Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

PubMed

Sun, Cheng-Jun; Zhang, Bangmin; Brewe, Dale L; Chen, Jing-Sheng; Chow, G M; Venkatesan, T; Heald, Steve M

2014-04-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

Ultrafast time-resolved X-ray absorption spectroscopy of ferrioxalate photolysis with a laser plasma X-ray source and microcalorimeter array

DOE PAGES

O’Neil, Galen C.; Miaja-Avila, Luis; Joe, Young Il; ...

2017-02-17

The detailed pathways of photoactivity on ultrafast time scales are a topic of contemporary interest. Using a tabletop apparatus based on a laser plasma X-ray source and an array of cryogenic microcalorimeter X-ray detectors, we measured a transient X-ray absorption spectrum during the ferrioxalate photoreduction reaction. With these high-efficiency detectors, we observe the Fe K edge move to lower energies and the amplitude of the extended X-ray absorption fine structure reduce, consistent with a photoreduction mechanism in which electron transfer precedes disassociation. We provide quantitative limits on the Fe–O bond length change. Lastly, we review potential improvements to our measurementmore » technique, highlighting the future potential of tabletop X-ray science using microcalorimeter sensors.« less

Ultrafast time-resolved X-ray absorption spectroscopy of ferrioxalate photolysis with a laser plasma X-ray source and microcalorimeter array

DOE Office of Scientific and Technical Information (OSTI.GOV)

O’Neil, Galen C.; Miaja-Avila, Luis; Joe, Young Il

The detailed pathways of photoactivity on ultrafast time scales are a topic of contemporary interest. Using a tabletop apparatus based on a laser plasma X-ray source and an array of cryogenic microcalorimeter X-ray detectors, we measured a transient X-ray absorption spectrum during the ferrioxalate photoreduction reaction. With these high-efficiency detectors, we observe the Fe K edge move to lower energies and the amplitude of the extended X-ray absorption fine structure reduce, consistent with a photoreduction mechanism in which electron transfer precedes disassociation. We provide quantitative limits on the Fe–O bond length change. Lastly, we review potential improvements to our measurementmore » technique, highlighting the future potential of tabletop X-ray science using microcalorimeter sensors.« less

Novel visualization studies of lignocellulosic oxidation chemistry by application of C-near edge X-ray absorption fine structure spectroscopy

Treesearch

Douglas G. Mancosky; Lucian A. Lucia; Hiroki Nanko; Sue Wirick; Alan W. Rudie; Robert Braun

2005-01-01

The research presented herein is the first attempt to probe the chemical nature of lignocellulosic samples by the application of carbon near edge X-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft X-ray technique that principally provides selective interrogation of discrete atomic moieties using photoelectrons of variable energies. The X1A beam...

Development of XAFS Into a Structure Determination Technique

NASA Astrophysics Data System (ADS)

Stern, E. A.

After the detection of diffraction of x-rays by M. Laue in 1912, the technique was soon applied to structure determination by Bragg within a year. On the other hand, although the edge steps in X-Ray absorption were discovered even earlier by Barkla and both the near edge (XANES) and extended X-Ray fine structure (EXAFS) past the edge were detected by 1929, it still took over 40 years to realize the structure information contained in this X-Ray absorption fine structure (XAFS). To understand this delay a brief historical review of the development of the scientific ideas that transformed XAFS into the premiere technique for local structure determination is given. The development includes both advances in theoretical understanding and calculational capabilities, and in experimental facilities, especially synchrotron radiation sources. The present state of the XAFS technique and its capabilities are summarized.

Diagnosis of a two wire X-pinch by X-ray absorption spectroscopy utilizing a doubly curved ellipsoidal crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cahill, A. D., E-mail: adc87@cornell.edu; Hoyt, C. L., E-mail: adc87@cornell.edu; Shelkovenko, T. A., E-mail: adc87@cornell.edu

2014-12-15

X-ray absorption spectroscopy is a powerful tool for the diagnosis of plasmas over a wide range of both temperature and density. However, such a measurement is often limited to probing plasmas with temperatures well below that of the x-ray source in order to avoid object plasma emission lines from obscuring important features of the absorption spectrum. This has excluded many plasmas from being investigated by this technique. We have developed an x-ray spectrometer that provides the ability to record absorption spectra from higher temperature plasmas than the usual approach allows without the risk of data contamination by line radiation emittedmore » by the plasma under study. This is accomplished using a doubly curved mica crystal which is bent both elliptically and cylindrically. We present here initial absorption spectra obtained from an aluminum x-pinch plasma.« less

A three-image algorithm for hard x-ray grating interferometry.

PubMed

Pelliccia, Daniele; Rigon, Luigi; Arfelli, Fulvia; Menk, Ralf-Hendrik; Bukreeva, Inna; Cedola, Alessia

2013-08-12

A three-image method to extract absorption, refraction and scattering information for hard x-ray grating interferometry is presented. The method comprises a post-processing approach alternative to the conventional phase stepping procedure and is inspired by a similar three-image technique developed for analyzer-based x-ray imaging. Results obtained with this algorithm are quantitatively comparable with phase-stepping. This method can be further extended to samples with negligible scattering, where only two images are needed to separate absorption and refraction signal. Thanks to the limited number of images required, this technique is a viable route to bio-compatible imaging with x-ray grating interferometer. In addition our method elucidates and strengthens the formal and practical analogies between grating interferometry and the (non-interferometric) diffraction enhanced imaging technique.

Thermal expansion behavior study of Co nanowire array with in situ x-ray diffraction and x-ray absorption fine structure techniques

NASA Astrophysics Data System (ADS)

Mo, Guang; Cai, Quan; Jiang, Longsheng; Wang, Wei; Zhang, Kunhao; Cheng, Weidong; Xing, Xueqing; Chen, Zhongjun; Wu, Zhonghua

2008-10-01

In situ x-ray diffraction and x-ray absorption fine structure techniques were used to study the structural change of ordered Co nanowire array with temperature. The results show that the Co nanowires are polycrystalline with hexagonal close packed structure without phase change up until 700 °C. A nonlinear thermal expansion behavior has been found and can be well described by a quadratic equation with the first-order thermal expansion coefficient of 4.3×10-6/°C and the second-order thermal expansion coefficient of 5.9×10-9/°C. The mechanism of this nonlinear thermal expansion behavior is discussed.

Report on the 18th International Conference on X-ray and Inner-Shell Processes (X99).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gemmell, D. S.; Physics

2000-01-01

The 18th conference of the series served as a forum for discussing fundamental issues in the field of x-ray and inner-shell processes and their application in various disciplines of science and technology. Special emphasis was given to the opportunities offered by modern synchrotron x-ray sources. The program included plenary talks, progress reports and poster presentations relating to new developments in the field of x-ray and inner-shell processes. The range of topics included: X-ray interactions with atoms, molecules, clusters, surfaces and solids; Decay processes for inner-shell vacancies; X-ray absorption and emission spectroscopy - Photoionization processes; Phenomena associated with highly charged ionsmore » and collisions with energetic particles; Electron-spin and -momentum spectroscopy; X-ray scattering and spectroscopy in the study of magnetic systems; Applications in materials science, biology, geosciences, and other disciplines; Elastic and inelastic x-ray scattering processes in atoms and molecules; Threshold phenomena (post-collision interaction, resonant Raman processes, etc.); Nuclear absorption and scattering of x-rays; 'Fourth-generation' x-ray sources; Processes exploiting the polarization and coherence properties of x-ray beams; Developments in experimental techniques (x-ray optics, temporal techniques, detectors); Microscopy, spectromicroscopy, and various imaging techniques; Non-linear processes and x-ray lasers; Ionization and excitation induced by charged particles and by x-rays; and Exotic atoms (including 'hollow' atoms and atoms that contain 'exotic' particles).« less

X-ray phase-contrast imaging

NASA Astrophysics Data System (ADS)

Endrizzi, Marco

2018-01-01

X-ray imaging is a standard tool for the non-destructive inspection of the internal structure of samples. It finds application in a vast diversity of fields: medicine, biology, many engineering disciplines, palaeontology and earth sciences are just few examples. The fundamental principle underpinning the image formation have remained the same for over a century: the X-rays traversing the sample are subjected to different amount of absorption in different parts of the sample. By means of phase-sensitive techniques it is possible to generate contrast also in relation to the phase shifts imparted by the sample and to extend the capabilities of X-ray imaging to those details that lack enough absorption contrast to be visualised in conventional radiography. A general overview of X-ray phase contrast imaging techniques is presented in this review, along with more recent advances in this fast evolving field and some examples of applications.

Measurements of K shell absorption jump factors and jump ratios using EDXRF technique

NASA Astrophysics Data System (ADS)

Kacal, Mustafa Recep; Han, İbrahim; Akman, Ferdi

2015-04-01

In the present work, the K-shell absorption jump factors and jump ratios for 30 elements between Ti ( Z = 22) and Er ( Z = 68) were measured by energy dispersive X-ray fluorescence (EDXRF) technique. The jump factors and jump ratios for these elements were determined by measuring the K shell fluorescence parameters such as the Kα X-ray production cross-sections, K shell fluorescence yields, Kβ-to- Kα X-rays intensity ratios, total atomic absorption cross sections and mass attenuation coefficients. The measurements were performed using an Am-241 radioactive point source and a Si (Li) detector in direct excitation and transmission experimental geometry. The results for jump factors and jump ratios were compared with theoretically calculated and the ones available in the literature.

Contrast enhancement of biological nanoporous materials with zinc oxide infiltration for electron and X-ray nanoscale microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ocola, L. E.; Sampathkumar, V.; Kasthuri, N.

Here, we show that using infiltration of ZnO metal oxide can be useful for high resolution imaging of biological samples in electron and X-ray microscopy. This method is compatible with standard fixation techniques that leave the sample dry, such as finishing with super critical CO 2 drying, or simple vacuum drying at 95°C. We demonstrate this technique can be applied on tooth and brain tissue samples. We also show that high resolution X-ray tomography can be performed on biological systems using Zn K edge (1s) absorption to enhance internal structures, and obtained the first nanoscale 10 KeV X-ray absorption imagesmore » of the interior regions of a tooth.« less

Contrast enhancement of biological nanoporous materials with zinc oxide infiltration for electron and X-ray nanoscale microscopy

DOE PAGES

Ocola, L. E.; Sampathkumar, V.; Kasthuri, N.; ...

2017-07-19

Here, we show that using infiltration of ZnO metal oxide can be useful for high resolution imaging of biological samples in electron and X-ray microscopy. This method is compatible with standard fixation techniques that leave the sample dry, such as finishing with super critical CO 2 drying, or simple vacuum drying at 95°C. We demonstrate this technique can be applied on tooth and brain tissue samples. We also show that high resolution X-ray tomography can be performed on biological systems using Zn K edge (1s) absorption to enhance internal structures, and obtained the first nanoscale 10 KeV X-ray absorption imagesmore » of the interior regions of a tooth.« less

Soft x-ray absorption spectroscopy of metalloproteins and high-valent metal-complexes at room temperature using free-electron lasers

PubMed Central

Kubin, Markus; Kern, Jan; Gul, Sheraz; Kroll, Thomas; Chatterjee, Ruchira; Löchel, Heike; Fuller, Franklin D.; Sierra, Raymond G.; Quevedo, Wilson; Weniger, Christian; Rehanek, Jens; Firsov, Anatoly; Laksmono, Hartawan; Weninger, Clemens; Alonso-Mori, Roberto; Nordlund, Dennis L.; Lassalle-Kaiser, Benedikt; Glownia, James M.; Krzywinski, Jacek; Moeller, Stefan; Turner, Joshua J.; Minitti, Michael P.; Dakovski, Georgi L.; Koroidov, Sergey; Kawde, Anurag; Kanady, Jacob S.; Tsui, Emily Y.; Suseno, Sandy; Han, Zhiji; Hill, Ethan; Taguchi, Taketo; Borovik, Andrew S.; Agapie, Theodor; Messinger, Johannes; Erko, Alexei; Föhlisch, Alexander; Bergmann, Uwe; Mitzner, Rolf; Yachandra, Vittal K.; Yano, Junko; Wernet, Philippe

2017-01-01

X-ray absorption spectroscopy at the L-edge of 3d transition metals provides unique information on the local metal charge and spin states by directly probing 3d-derived molecular orbitals through 2p-3d transitions. However, this soft x-ray technique has been rarely used at synchrotron facilities for mechanistic studies of metalloenzymes due to the difficulties of x-ray-induced sample damage and strong background signals from light elements that can dominate the low metal signal. Here, we combine femtosecond soft x-ray pulses from a free-electron laser with a novel x-ray fluorescence-yield spectrometer to overcome these difficulties. We present L-edge absorption spectra of inorganic high-valent Mn complexes (Mn ∼ 6–15 mmol/l) with no visible effects of radiation damage. We also present the first L-edge absorption spectra of the oxygen evolving complex (Mn4CaO5) in Photosystem II (Mn < 1 mmol/l) at room temperature, measured under similar conditions. Our approach opens new ways to study metalloenzymes under functional conditions. PMID:28944255

Soft x-ray absorption spectroscopy of metalloproteins and high-valent metal-complexes at room temperature using free-electron lasers

DOE PAGES

Kubin, Markus; Kern, Jan; Gul, Sheraz; ...

2017-09-01

X-ray absorption spectroscopy at the L-edge of 3d transition metals provides unique information on the local metal charge and spin states by directly probing 3d-derived molecular orbitals through 2p-3d transitions. But, this soft x-ray technique has been rarely used at synchrotron facilities for mechanistic studies of metalloenzymes due to the difficulties of x-ray-induced sample damage and strong background signals from light elements that can dominate the low metal signal. Here, we combine femtosecond soft x-ray pulses from a free-electron laser with a novel x-ray fluorescence-yield spectrometer to overcome these difficulties. We present L-edge absorption spectra of inorganic high-valent Mn complexesmore » (Mn ~ 6-15 mmol/l) with no visible effects of radiation damage. We then present the first L-edge absorption spectra of the oxygen evolving complex (Mn 4 CaO 5 ) in Photosystem II (Mn < 1 mmol/l) at room temperature, measured under similar conditions. Our approach opens new ways to study metalloenzymes under functional conditions.« less

Quantitative Electron Probe Microanalysis: State of the Art

NASA Technical Reports Server (NTRS)

Carpernter, P. K.

2005-01-01

Quantitative electron-probe microanalysis (EPMA) has improved due to better instrument design and X-ray correction methods. Design improvement of the electron column and X-ray spectrometer has resulted in measurement precision that exceeds analytical accuracy. Wavelength-dispersive spectrometer (WDS) have layered-dispersive diffraction crystals with improved light-element sensitivity. Newer energy-dispersive spectrometers (EDS) have Si-drift detector elements, thin window designs, and digital processing electronics with X-ray throughput approaching that of WDS Systems. Using these systems, digital X-ray mapping coupled with spectrum imaging is a powerful compositional mapping tool. Improvements in analytical accuracy are due to better X-ray correction algorithms, mass absorption coefficient data sets,and analysis method for complex geometries. ZAF algorithms have ban superceded by Phi(pz) algorithms that better model the depth distribution of primary X-ray production. Complex thin film and particle geometries are treated using Phi(pz) algorithms, end results agree well with Monte Carlo simulations. For geological materials, X-ray absorption dominates the corretions end depends on the accuracy of mass absorption coefficient (MAC) data sets. However, few MACs have been experimentally measured, and the use of fitted coefficients continues due to general success of the analytical technique. A polynomial formulation of the Bence-Albec alpha-factor technique, calibrated using Phi(pz) algorithms, is used to critically evaluate accuracy issues and can be also be used for high 2% relative and is limited by measurement precision for ideal cases, but for many elements the analytical accuracy is unproven. The EPMA technique has improved to the point where it is frequently used instead of the petrogaphic microscope for reconnaissance work. Examples of stagnant research areas are: WDS detector design characterization of calibration standards, and the need for more complete treatment of the continuum X-ray fluorescence correction.

Development of an x-ray prism for analyzer based imaging systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bewer, Brian; Chapman, Dean

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP)more » was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.« less

Development of an x-ray prism for analyzer based imaging systems

NASA Astrophysics Data System (ADS)

Bewer, Brian; Chapman, Dean

2010-08-01

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP) was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.

Development of an x-ray prism for analyzer based imaging systems.

PubMed

Bewer, Brian; Chapman, Dean

2010-08-01

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP) was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.

From synchrotron radiation to lab source: advanced speckle-based X-ray imaging using abrasive paper

NASA Astrophysics Data System (ADS)

Wang, Hongchang; Kashyap, Yogesh; Sawhney, Kawal

2016-02-01

X-ray phase and dark-field imaging techniques provide complementary and inaccessible information compared to conventional X-ray absorption or visible light imaging. However, such methods typically require sophisticated experimental apparatus or X-ray beams with specific properties. Recently, an X-ray speckle-based technique has shown great potential for X-ray phase and dark-field imaging using a simple experimental arrangement. However, it still suffers from either poor resolution or the time consuming process of collecting a large number of images. To overcome these limitations, in this report we demonstrate that absorption, dark-field, phase contrast, and two orthogonal differential phase contrast images can simultaneously be generated by scanning a piece of abrasive paper in only one direction. We propose a novel theoretical approach to quantitatively extract the above five images by utilising the remarkable properties of speckles. Importantly, the technique has been extended from a synchrotron light source to utilise a lab-based microfocus X-ray source and flat panel detector. Removing the need to raster the optics in two directions significantly reduces the acquisition time and absorbed dose, which can be of vital importance for many biological samples. This new imaging method could potentially provide a breakthrough for numerous practical imaging applications in biomedical research and materials science.

Near Edge X-Ray Absorption and X-Ray Photoelectron Diffraction Studies of the Structural Environment of Ge-Si Systems

NASA Astrophysics Data System (ADS)

Castrucci, P.; Gunnella, R.; Pinto, N.; Bernardini, R.; de Crescenzi, M.; Sacchi, M.

Near edge X-ray absorption spectroscopy (XAS), X-ray photoelectron diffraction (XPD) and Auger electron diffraction (AED) are powerful techniques for the qualitative study of the structural and electronic properties of several systems. The recent development of a multiple scattering approach to simulating experimental spectra opened a friendly way to the study of structural environments of solids and surfaces. This article reviews recent X-ray absorption experiments using synchrotron radiation which were performed at Ge L edges and core level electron diffraction measurements obtained using a traditional X-ray source from Ge core levels for ultrathin Ge films deposited on silicon substrates. Thermodynamics and surface reconstruction have been found to play a crucial role in the first stages of Ge growth on Si(001) and Si(111) surfaces. Both techniques show the occurrence of intermixing processes even for room-temperature-grown Ge/Si(001) samples and give a straightforward measurement of the overlayer tetragonal distortion. The effects of Sb as a surfactant on the Ge/Si(001) interface have also been investigated. In this case, evidence of layer-by-layer growth of the fully strained Ge overlayer with a reduced intermixing is obtained when one monolayer of Sb is predeposited on the surface.

X-ray absorption fine structure and X-ray excited optical luminescence studies of II-VI semiconducting nanostructures

NASA Astrophysics Data System (ADS)

Murphy, Michael Wayne

2010-06-01

Various II-VI semiconducting nanomaterials such as ZnO-ZnS nanoribbons (NRs), CdSxSe1-x nanostructures, ZnS:Mn NRs, ZnS:Mn,Eu nanoprsims (NPs), ZnO:Mn nanopowders, and ZnO:Co nanopowders were synthesized for study. These materials were characterized by techniques such as scanning electron microscopy, transmission electron microscopy, element dispersive X-ray spectroscopy, selected area electron diffraction, and X-ray diffraction. The electronic and optical properties of these nanomaterials were studied by X-ray absorption fine structure (XAFS) spectroscopy and X-ray excited optical luminescence (XEOL) techniques, using tuneable soft X-rays from a synchrotron light source. The complementary nature ofthe XAFS and XEOL techniques give site, element and chemical specific measurements which allow a better understanding of the interplay and role of each element in the system. Chemical vapour deposition (CVD) of ZnS powder in a limited oxygen environment resulted in side-by-side biaxial ZnO-ZnS NR heterostructures. The resulting NRs contained distinct wurtzite ZnS and wurtzite ZnO components with widths of 10--100 nm and 20 --500 nm, respectively and a uniform interface region of 5-15 nm. XAFS and XEOL measurements revealed the luminescence of ZnO-ZnS NRs is from the ZnO component. The luminescence of CdSxSe1-x nanostructures is shown to be dependent on the S to Se ratio, with the band-gap emission being tunable between that of pure CdS and CdSe. Excitation of the CdSxSe 1-x nanostructures by X-ray in XEOL has revealed new de-excitation channels which show a defect emission band not seen by laser excitation. CVD of Mn2+ doped ZnS results in nanostructures with luminescence dominated by the yellow Mn2+ emission due to energy transfer from the ZnS host to the Mn dopant sites. The addition of EuCl3 to the reactants in the CVD process results in a change in morphology from NR to NP. Zn1-xMnxO and Zn1-xCOxO nanopowders were prepared by sol-gel methods at dopant concentrations of 0, 1,3, and 10% and annealed at 400, 600 and 800°C in air. XAFS spectra show that low dopant concentrations and low processing temperatures limit the amount of secondary phase formation. The nanopowders did not show roomtemperature ferromagnetism and increased secondary phase formation increases the paramagnetic character of the hysteresis curves at 5°K. Keywords: X-ray absorption fine structures (XAFS), X-ray absorption near-edge structures (XANES), extended X-ray absorption fine structure (EXAFS), X-ray absorption spectroscopy(XAS), X-ray excited optical luminescence (XEOL), time-resolved, II-VI semiconductors, nanostructure, nanomaterial, nanoribbon, nanowire, nanopartic1e, heterostructure, ZnO, ZnS, ZnO-ZnS, CdS, CdSe, CdSSe, ZnO:Mn, ZnO:Co, ZnS:Mn, dilute magnetic semiconductor (DMS), dilute magnetic oxide (DMO), spintronics, magnetism, paramagnetism, ferromagnetism.

Quantitative X-ray Differential Interference Contrast Microscopy

NASA Astrophysics Data System (ADS)

Nakamura, Takashi

Full-field soft x-ray microscopes are widely used in many fields of sciences. Advances in nanofabrication technology enabled short wavelength focusing elements with significantly improved spatial resolution. In the soft x-ray spectral region, samples as small as 12 nm can be resolved using micro zone-plates as the objective lens. In addition to conventional x-ray microscopy in which x-ray absorption difference provides the image contrast, phase contrast mechanisms such as differential phase contrast (DIC) and Zernike phase contrast have also been demonstrated These phase contrast imaging mechanisms are especially attractive at the x-ray wavelengths where phase contrast of most materials is typically 10 times stronger than the absorption contrast. With recent progresses in plasma-based x- ray sources and increasing accessibility to synchrotron user facilities, x-ray microscopes are quickly becoming standard measurement equipment in the laboratory. To further the usefulness of x-ray DIC microscopy this thesis explicitly addresses three known issues with this imaging modality by introducing new techniques and devices First, as opposed to its visible-light counterpart, no quantitative phase imaging technique exists for x-ray DIC microscopy. To address this issue, two nanoscale x-ray quantitative phase imaging techniques, using exclusive OR (XOR) patterns and zone-plate doublets, respectively, are proposed. Unlike existing x-ray quantitative phase imaging techniques such as Talbot interferometry and ptychography, no dedicated experimental setups or stringent illumination coherence are needed for quantitative phase retrieval. Second, to the best of our knowledge, no quantitative performance characterization of DIC microscopy exists to date. Therefore the imaging system's response to sample's spatial frequency is not known In order to gain in-depth understanding of this imaging modality, performance of x-ray DIC microscopy is quantified using modulation transfer function. A new illumination apparatus required for the transfer function analysis under partially coherent illumination is also proposed. Such a characterization is essential for a proper selection of DIC optics for various transparent samples under study. Finally, optical elements used for x-ray DIC microscopy are highly absorptive and high brilliance x-ray sources such as synchrotrons are generally needed for image contrast. To extend the use of x-ray DIC microscopy to a wider variety of applications, a high efficiency large numerical aperture optical element consisting of high reflective Bragg reflectors is proposed. Using Bragg reflectors, which have 70% ˜99% reflectivity at extreme ultraviolet and soft x-rays for all angles of glancing incidence, the first order focusing efficiency is expected to increase by ˜ 8 times compared to that of a typical Fresnel zone-plate. This thesis contributes to current nanoscale x-ray phase contrast imaging research and provides new insights for biological, material, and magnetic sciences

X-ray Scatter Imaging of Hepatocellular Carcinoma in a Mouse Model Using Nanoparticle Contrast Agents

NASA Astrophysics Data System (ADS)

Rand, Danielle; Derdak, Zoltan; Carlson, Rolf; Wands, Jack R.; Rose-Petruck, Christoph

2015-10-01

Hepatocellular carcinoma (HCC) is one of the most common malignant tumors worldwide and is almost uniformly fatal. Current methods of detection include ultrasound examination and imaging by CT scan or MRI; however, these techniques are problematic in terms of sensitivity and specificity, and the detection of early tumors (<1 cm diameter) has proven elusive. Better, more specific, and more sensitive detection methods are therefore urgently needed. Here we discuss the application of a newly developed x-ray imaging technique called Spatial Frequency Heterodyne Imaging (SFHI) for the early detection of HCC. SFHI uses x-rays scattered by an object to form an image and is more sensitive than conventional absorption-based x-radiography. We show that tissues labeled in vivo with gold nanoparticle contrast agents can be detected using SFHI. We also demonstrate that directed targeting and SFHI of HCC tumors in a mouse model is possible through the use of HCC-specific antibodies. The enhanced sensitivity of SFHI relative to currently available techniques enables the x-ray imaging of tumors that are just a few millimeters in diameter and substantially reduces the amount of nanoparticle contrast agent required for intravenous injection relative to absorption-based x-ray imaging.

X-ray absorption and reflection as probes of the GaN conduction bands: Theory and experiments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lambrecht, W.R.L.; Rashkeev, S.N.; Segall, B.

1997-04-01

X-ray absorption measurements are a well-known probe of the unoccupied states in a material. The same information can be obtained by using glancing angle X-ray reflectivity. In spite of several existing band structure calculations of the group III nitrides and previous optical studies in UV range, a direct probe of their conduction band densities of states is of interest. The authors performed a joint experimental and theoretical investigation using both of these experimental techniques for wurtzite GaN.

New consistency tests for high-accuracy measurements of X-ray mass attenuation coefficients by the X-ray extended-range technique.

PubMed

Chantler, C T; Islam, M T; Rae, N A; Tran, C Q; Glover, J L; Barnea, Z

2012-03-01

An extension of the X-ray extended-range technique is described for measuring X-ray mass attenuation coefficients by introducing absolute measurement of a number of foils - the multiple independent foil technique. Illustrating the technique with the results of measurements for gold in the 38-50 keV energy range, it is shown that its use enables selection of the most uniform and well defined of available foils, leading to more accurate measurements; it allows one to test the consistency of independently measured absolute values of the mass attenuation coefficient with those obtained by the thickness transfer method; and it tests the linearity of the response of the counter and counting chain throughout the range of X-ray intensities encountered in a given experiment. In light of the results for gold, the strategy to be ideally employed in measuring absolute X-ray mass attenuation coefficients, X-ray absorption fine structure and related quantities is discussed.

X-ray grating interferometry at photon energies over 180 keV

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ruiz-Yaniz, M., E-mail: maite.ruiz-yaniz@esrf.fr; Lehrstuhl für Biomedizinische Physik, Physik-Department and Institut für Medizintechnik, Technische Universität München, James-Franck-Str. 1, 85748 Garching; Koch, F.

2015-04-13

We report on the implementation and characterization of grating interferometry operating at an x-ray energy of 183 keV. With the possibility to use this technique at high x-ray energies, bigger specimens could be studied in a quantitative way. Also, imaging strongly absorbing specimens will benefit from the advantages of the phase and dark-field signals provided by grating interferometry. However, especially at these high photon energies the performance of the absorption grating becomes a key point on the quality of the system, because the grating lines need to keep their small width of a couple of micrometers and exhibit a greater heightmore » of hundreds of micrometers. The performance of high aspect ratio absorption gratings fabricated with different techniques is discussed. Further, a dark-field image of an alkaline multicell battery highlights the potential of high energy x-ray grating based imaging.« less

Biological X-ray absorption spectroscopy (BioXAS): a valuable tool for the study of trace elements in the life sciences.

PubMed

Strange, Richard W; Feiters, Martin C

2008-10-01

Using X-ray absorption spectroscopy (XAS) the binding modes (type and number of ligands, distances and geometry) and oxidation states of metals and other trace elements in crystalline as well as non-crystalline samples can be revealed. The method may be applied to biological systems as a 'stand-alone' technique, but it is particularly powerful when used alongside other X-ray and spectroscopic techniques and computational approaches. In this review, we highlight how biological XAS is being used in concert with crystallography, spectroscopy and computational chemistry to study metalloproteins in crystals, and report recent applications on relatively rare trace elements utilised by living organisms and metals involved in neurodegenerative diseases.

Surface degradation of uranium tetrafluoride

DOE PAGES

Tobin, J. G.; Duffin, A. M.; Yu, S. -W.; ...

2017-05-01

A detailed analysis of a single crystal of uranium tetrafluoride has been carried out. The techniques include x-ray absorption spectroscopy, as well as x-ray photoelectron spectroscopy and x-ray emission spectroscopy. Evidence will be presented for the presence of a uranyl species, possibly UO 2F 2, as a product of, or participant in the surface degradation.

Optimization-Based Approach for Joint X-Ray Fluorescence and Transmission Tomographic Inversion

DOE Office of Scientific and Technical Information (OSTI.GOV)

Di, Zichao; Leyffer, Sven; Wild, Stefan M.

2016-01-01

Fluorescence tomographic reconstruction, based on the detection of photons coming from fluorescent emission, can be used for revealing the internal elemental composition of a sample. On the other hand, conventional X-ray transmission tomography can be used for reconstructing the spatial distribution of the absorption coefficient inside a sample. In this work, we integrate both X-ray fluorescence and X-ray transmission data modalities and formulate a nonlinear optimization-based approach for reconstruction of the elemental composition of a given object. This model provides a simultaneous reconstruction of both the quantitative spatial distribution of all elements and the absorption effect in the sample. Mathematicallymore » speaking, we show that compared with the single-modality inversion (i.e., the X-ray transmission or fluorescence alone), the joint inversion provides a better-posed problem, which implies a better recovery. Therefore, the challenges in X-ray fluorescence tomography arising mainly from the effects of self-absorption in the sample are partially mitigated. The use of this technique is demonstrated on the reconstruction of several synthetic samples.« less

MMX-I: data-processing software for multimodal X-ray imaging and tomography.

PubMed

Bergamaschi, Antoine; Medjoubi, Kadda; Messaoudi, Cédric; Marco, Sergio; Somogyi, Andrea

2016-05-01

A new multi-platform freeware has been developed for the processing and reconstruction of scanning multi-technique X-ray imaging and tomography datasets. The software platform aims to treat different scanning imaging techniques: X-ray fluorescence, phase, absorption and dark field and any of their combinations, thus providing an easy-to-use data processing tool for the X-ray imaging user community. A dedicated data input stream copes with the input and management of large datasets (several hundred GB) collected during a typical multi-technique fast scan at the Nanoscopium beamline and even on a standard PC. To the authors' knowledge, this is the first software tool that aims at treating all of the modalities of scanning multi-technique imaging and tomography experiments.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Di, Zichao; Leyffer, Sven; Wild, Stefan M.

Fluorescence tomographic reconstruction, based on the detection of photons coming from fluorescent emission, can be used for revealing the internal elemental composition of a sample. On the other hand, conventional X-ray transmission tomography can be used for reconstructing the spatial distribution of the absorption coefficient inside a sample. In this work, we integrate both X-ray fluorescence and X-ray transmission data modalities and formulate a nonlinear optimization-based approach for reconstruction of the elemental composition of a given object. This model provides a simultaneous reconstruction of both the quantitative spatial distribution of all elements and the absorption effect in the sample. Mathematicallymore » speaking, we show that compared with the single-modality inversion (i.e., the X-ray transmission or fluorescence alone), the joint inversion provides a better-posed problem, which implies a better recovery. Therefore, the challenges in X-ray fluorescence tomography arising mainly from the effects of self-absorption in the sample are partially mitigated. The use of this technique is demonstrated on the reconstruction of several synthetic samples.« less

Toward picosecond time-resolved X-ray absorption studies of interfacial photochemistry

NASA Astrophysics Data System (ADS)

Gessner, Oliver; Mahl, Johannes; Neppl, Stefan

2016-05-01

We report on the progress toward developing a novel picosecond time-resolved transient X-ray absorption spectroscopy (TRXAS) capability for time-domain studies of interfacial photochemistry. The technique is based on the combination of a high repetition rate picosecond laser system with a time-resolved X-ray fluorescent yield setup that may be used for the study of radiation sensitive materials and X-ray spectroscopy compatible photoelectrochemical (PEC) cells. The mobile system is currently deployed at the Advanced Light Source (ALS) and may be used in all operating modes (two-bunch and multi-bunch) of the synchrotron. The use of a time-stamping technique enables the simultaneous recording of TRXAS spectra with delays between the exciting laser pulses and the probing X-ray pulses spanning picosecond to nanosecond temporal scales. First results are discussed that demonstrate the viability of the method to study photoinduced dynamics in transition metal-oxide semiconductor (SC) samples under high vacuum conditions and at SC-liquid electrolyte interfaces during photoelectrochemical water splitting. Opportunities and challenges are outlined to capture crucial short-lived intermediates of photochemical processes with the technique. This work was supported by the Department of Energy Office of Science Early Career Research Program.

Mass density images from the diffraction enhanced imaging technique.

PubMed

Hasnah, M O; Parham, C; Pisano, E D; Zhong, Z; Oltulu, O; Chapman, D

2005-02-01

Conventional x-ray radiography measures the projected x-ray attenuation of an object. It requires attenuation differences to obtain contrast of embedded features. In general, the best absorption contrast is obtained at x-ray energies where the absorption is high, meaning a high absorbed dose. Diffraction-enhanced imaging (DEI) derives contrast from absorption, refraction, and extinction. The refraction angle image of DEI visualizes the spatial gradient of the projected electron density of the object. The projected electron density often correlates well with the projected mass density and projected absorption in soft-tissue imaging, yet the mass density is not an "energy"-dependent property of the object, as is the case of absorption. This simple difference can lead to imaging with less x-ray exposure or dose. In addition, the mass density image can be directly compared (i.e., a signal-to-noise comparison) with conventional radiography. We present the method of obtaining the mass density image, the results of experiments in which comparisons are made with radiography, and an application of the method to breast cancer imaging.

Tracking reaction dynamics in solution by pump-probe X-ray absorption spectroscopy and X-ray liquidography (solution scattering).

PubMed

Kim, Jeongho; Kim, Kyung Hwan; Oang, Key Young; Lee, Jae Hyuk; Hong, Kiryong; Cho, Hana; Huse, Nils; Schoenlein, Robert W; Kim, Tae Kyu; Ihee, Hyotcherl

2016-03-07

Characterization of transient molecular structures formed during chemical and biological processes is essential for understanding their mechanisms and functions. Over the last decade, time-resolved X-ray liquidography (TRXL) and time-resolved X-ray absorption spectroscopy (TRXAS) have emerged as powerful techniques for molecular and electronic structural analysis of photoinduced reactions in the solution phase. Both techniques make use of a pump-probe scheme that consists of (1) an optical pump pulse to initiate a photoinduced process and (2) an X-ray probe pulse to monitor changes in the molecular structure as a function of time delay between pump and probe pulses. TRXL is sensitive to changes in the global molecular structure and therefore can be used to elucidate structural changes of reacting solute molecules as well as the collective response of solvent molecules. On the other hand, TRXAS can be used to probe changes in both local geometrical and electronic structures of specific X-ray-absorbing atoms due to the element-specific nature of core-level transitions. These techniques are complementary to each other and a combination of the two methods will enhance the capability of accurately obtaining structural changes induced by photoexcitation. Here we review the principles of TRXL and TRXAS and present recent application examples of the two methods for studying chemical and biological processes in solution. Furthermore, we briefly discuss the prospect of using X-ray free electron lasers for the two techniques, which will allow us to keep track of structural dynamics on femtosecond time scales in various solution-phase molecular reactions.

X-ray Absorption Spectroscopy Characterization of Electrochemical Processes in Renewable Energy Storage and Conversion Devices

DOE Office of Scientific and Technical Information (OSTI.GOV)

Farmand, Maryam

2013-05-19

The development of better energy conversion and storage devices, such as fuel cells and batteries, is crucial for reduction of our global carbon footprint and improving the quality of the air we breathe. However, both of these technologies face important challenges. The development of lower cost and better electrode materials, which are more durable and allow more control over the electrochemical reactions occurring at the electrode/electrolyte interface, is perhaps most important for meeting these challenges. Hence, full characterization of the electrochemical processes that occur at the electrodes is vital for intelligent design of more energy efficient electrodes. X-ray absorption spectroscopymore » (XAS) is a short-range order, element specific technique that can be utilized to probe the processes occurring at operating electrode surfaces, as well for studying the amorphous materials and nano-particles making up the electrodes. It has been increasingly used in recent years to study fuel cell catalysts through application of the and #916; and mgr; XANES technique, in combination with the more traditional X-ray Absorption Near Edge Structure (XANES) and Extended X-ray Absorption Fine Structure (EXAFS) techniques. The and #916; and mgr; XANES data analysis technique, previously developed and applied to heterogeneous catalysts and fuel cell electrocatalysts by the GWU group, was extended in this work to provide for the first time space resolved adsorbate coverages on both electrodes of a direct methanol fuel cell. Even more importantly, the and #916; and mgr; technique was applied for the first time to battery relevant materials, where bulk properties such as the oxidation state and local geometry of a cathode are followed.« less

X-ray scatter imaging of hepatocellular carcinoma in a mouse model using nanoparticle contrast agents

DOE PAGES

Rand, Danielle; Derdak, Zoltan; Carlson, Rolf; ...

2015-10-29

Hepatocellular carcinoma (HCC) is one of the most common malignant tumors worldwide and is almost uniformly fatal. Current methods of detection include ultrasound examination and imaging by CT scan or MRI; however, these techniques are problematic in terms of sensitivity and specificity, and the detection of early tumors (<1 cm diameter) has proven elusive. Better, more specific, and more sensitive detection methods are therefore urgently needed. Here we discuss the application of a newly developed x-ray imaging technique called Spatial Frequency Heterodyne Imaging (SFHI) for the early detection of HCC. SFHI uses x-rays scattered by an object to form anmore » image and is more sensitive than conventional absorption-based x-radiography. We show that tissues labeled in vivo with gold nanoparticle contrast agents can be detected using SFHI. We also demonstrate that directed targeting and SFHI of HCC tumors in a mouse model is possible through the use of HCC-specific antibodies. As a result, the enhanced sensitivity of SFHI relative to currently available techniques enables the x-ray imaging of tumors that are just a few millimeters in diameter and substantially reduces the amount of nanoparticle contrast agent required for intravenous injection relative to absorption-based x-ray imaging.« less

Determination of copper binding in Pseudomonas putida CZ1 by chemical modifications and X-ray absorption spectroscopy.

PubMed

Chen, XinCai; Shi, JiYan; Chen, YingXu; Xu, XiangHua; Chen, LiTao; Wang, Hui; Hu, TianDou

2007-03-01

Previously performed studies have shown that Pseudomonas putida CZ1 biomass can bind an appreciable amount of Cu(II) and Zn(II) ions from aqueous solutions. The mechanisms of Cu- and Zn-binding by P. putida CZ1 were ascertained by chemical modifications of the biomass followed by Fourier transform infrared and X-ray absorption spectroscopic analyses of the living or nonliving cells. A dramatic decrease in Cu(II)- and Zn(II)-binding resulted after acidic methanol esterification of the nonliving cells, indicating that carboxyl functional groups play an important role in the binding of metal to the biomaterial. X-ray absorption spectroscopy was used to determine the speciation of Cu ions bound by living and nonliving cells, as well as to elucidate which functional groups were involved in binding of the Cu ions. The X-ray absorption near-edge structure spectra analysis showed that the majority of the Cu was bound in both samples as Cu(II). The fitting results of Cu K-edge extended X-ray absorption fine structure spectra showed that N/O ligands dominated in living and nonliving cells. Therefore, by combining different techniques, our results indicate that carboxyl functional groups are the major ligands responsible for the metal binding in P. putida CZ1.

Quantitative X-ray dark-field and phase tomography using single directional speckle scanning technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Hongchang, E-mail: hongchang.wang@diamond.ac.uk; Kashyap, Yogesh; Sawhney, Kawal

2016-03-21

X-ray dark-field contrast tomography can provide important supplementary information inside a sample to the conventional absorption tomography. Recently, the X-ray speckle based technique has been proposed to provide qualitative two-dimensional dark-field imaging with a simple experimental arrangement. In this letter, we deduce a relationship between the second moment of scattering angle distribution and cross-correlation degradation of speckle and establish a quantitative basis of X-ray dark-field tomography using single directional speckle scanning technique. In addition, the phase contrast images can be simultaneously retrieved permitting tomographic reconstruction, which yields enhanced contrast in weakly absorbing materials. Such complementary tomography technique can allow systematicmore » investigation of complex samples containing both soft and hard materials.« less

MMX-I: data-processing software for multimodal X-ray imaging and tomography

PubMed Central

Bergamaschi, Antoine; Medjoubi, Kadda; Messaoudi, Cédric; Marco, Sergio; Somogyi, Andrea

2016-01-01

A new multi-platform freeware has been developed for the processing and reconstruction of scanning multi-technique X-ray imaging and tomography datasets. The software platform aims to treat different scanning imaging techniques: X-ray fluorescence, phase, absorption and dark field and any of their combinations, thus providing an easy-to-use data processing tool for the X-ray imaging user community. A dedicated data input stream copes with the input and management of large datasets (several hundred GB) collected during a typical multi-technique fast scan at the Nanoscopium beamline and even on a standard PC. To the authors’ knowledge, this is the first software tool that aims at treating all of the modalities of scanning multi-technique imaging and tomography experiments. PMID:27140159

Applications of synchrotron-based spectroscopic techniques in studying nucleic acids and nucleic acid-functionalized nanomaterials

PubMed Central

Wu, Peiwen; Yu, Yang; McGhee, Claire E.; Tan, Li Huey

2014-01-01

In this review, we summarize recent progresses in the application of synchrotron-based spectroscopic techniques for nucleic acid research that takes advantage of high-flux and high-brilliance electromagnetic radiation from synchrotron sources. The first section of the review focuses on the characterization of the structure and folding processes of nucleic acids using different types of synchrotron-based spectroscopies, such as X-ray absorption spectroscopy, X-ray emission spectroscopy, X-ray photoelectron spectroscopy, synchrotron radiation circular dichroism, X-ray footprinting and small-angle X-ray scattering. In the second section, the characterization of nucleic acid-based nanostructures, nucleic acid-functionalized nanomaterials and nucleic acid-lipid interactions using these spectroscopic techniques is summarized. Insights gained from these studies are described and future directions of this field are also discussed. PMID:25205057

Applications of synchrotron-based spectroscopic techniques in studying nucleic acids and nucleic acid-functionalized nanomaterials

DOE PAGES

Wu, Peiwen; Yu, Yang; McGhee, Claire E.; ...

2014-09-10

In this paper, we summarize recent progress in the application of synchrotron-based spectroscopic techniques for nucleic acid research that takes advantage of high-flux and high-brilliance electromagnetic radiation from synchrotron sources. The first section of the review focuses on the characterization of the structure and folding processes of nucleic acids using different types of synchrotron-based spectroscopies, such as X-ray absorption spectroscopy, X-ray emission spectroscopy, X-ray photoelectron spectroscopy, synchrotron radiation circular dichroism, X-ray footprinting and small-angle X-ray scattering. In the second section, the characterization of nucleic acid-based nanostructures, nucleic acid-functionalized nanomaterials and nucleic acid-lipid interactions using these spectroscopic techniques is summarized. Insightsmore » gained from these studies are described and future directions of this field are also discussed.« less

Time-resolved x-ray absorption spectroscopy: Watching atoms dance

NASA Astrophysics Data System (ADS)

Milne, Chris J.; Pham, Van-Thai; Gawelda, Wojciech; van der Veen, Renske M.; El Nahhas, Amal; Johnson, Steven L.; Beaud, Paul; Ingold, Gerhard; Lima, Frederico; Vithanage, Dimali A.; Benfatto, Maurizio; Grolimund, Daniel; Borca, Camelia; Kaiser, Maik; Hauser, Andreas; Abela, Rafael; Bressler, Christian; Chergui, Majed

2009-11-01

The introduction of pump-probe techniques to the field of x-ray absorption spectroscopy (XAS) has allowed the monitoring of both structural and electronic dynamics of disordered systems in the condensed phase with unprecedented accuracy, both in time and in space. We present results on the electronically excited high-spin state structure of an Fe(II) molecular species, [FeII(bpy)3]2+, in aqueous solution, resolving the Fe-N bond distance elongation as 0.2 Å. In addition an analysis technique using the reduced χ2 goodness of fit between FEFF EXAFS simulations and the experimental transient absorption signal in energy space has been successfully tested as a function of excited state population and chemical shift, demonstrating its applicability in situations where the fractional excited state population cannot be determined through other measurements. Finally by using a novel ultrafast hard x-ray 'slicing' source the question of how the molecule relaxes after optical excitation has been successfully resolved using femtosecond XANES.

Review of Canadian Light Source facilities for biological applications

NASA Astrophysics Data System (ADS)

Grochulski, Pawel; Fodje, Michel; Labiuk, Shaun; Wysokinski, Tomasz W.; Belev, George; Korbas, Malgorzata; Rosendahl, Scott M.

2017-11-01

The newly-created Biological and Life Sciences Department at the Canadian Light Source (CLS) encompasses four sets of beamlines devoted to biological studies ranging in scope from the atomic scale to cells, tissues and whole organisms. The Canadian Macromolecular Crystallography Facility (CMCF) consists of two beamlines devoted primarily to crystallographic studies of proteins and other macromolecules. The Mid-Infrared Spectromicroscopy (Mid-IR) beamline focusses on using infrared energy to obtain biochemical, structural and dynamical information about biological systems. The Bio-Medical Imaging and Therapy (BMIT) facility consists of two beamlines devoted to advanced imaging and X-ray therapy techniques. The Biological X-ray Absorption Spectroscopy (BioXAS) facility is being commissioned and houses three beamlines devoted to X-ray absorption spectroscopy and multi-mode X-ray fluorescence imaging. Together, these beamlines provide CLS Users with a powerful array of techniques to study today's most pressing biological questions. We describe these beamlines along with their current powerful features and envisioned future capabilities.

Simultaneous fast scanning XRF, dark field, phase-, and absorption contrast tomography

NASA Astrophysics Data System (ADS)

Medjoubi, Kadda; Bonissent, Alain; Leclercq, Nicolas; Langlois, Florent; Mercère, Pascal; Somogyi, Andrea

2013-09-01

Scanning hard X-ray nanoprobe imaging provides a unique tool for probing specimens with high sensitivity and large penetration depth. Moreover, the combination of complementary techniques such as X-ray fluorescence, absorption, phase contrast and dark field imaging gives complete quantitative information on the sample structure, composition and chemistry. The multi-technique "FLYSCAN" data acquisition scheme developed at Synchrotron SOLEIL permits to perform fast continuous scanning imaging and as such makes scanning tomography techniques feasible in a time-frame well-adapted to typical user experiments. Here we present the recent results of simultaneous fast scanning multi-technique tomography performed at Soleil. This fast scanning scheme will be implemented at the Nanoscopium beamline for large field of view 2D and 3D multimodal imaging.

Parametric studies and characterization measurements of x-ray lithography mask membranes

NASA Astrophysics Data System (ADS)

Wells, Gregory M.; Chen, Hector T. H.; Engelstad, Roxann L.; Palmer, Shane R.

1991-08-01

The techniques used in the experimental characterization of thin membranes are considered for their potential use as mask blanks for x-ray lithography. Among the parameters of interest for this evaluation are the film's stress, fracture strength, uniformity of thickness, absorption in the x-ray and visible spectral regions and the modulus and grain structure of the material. The experimental techniques used for measuring these properties are described. The accuracy and applicability of the assumptions used to derive the formulas that relate the experimental measurements to the parameters of interest are considered. Experimental results for silicon carbide and diamond films are provided. Another characteristic needed for an x-ray mask carrier is radiation stability. The number of x-ray exposures expected to be performed in the lifetime of an x-ray mask on a production line is on the order of 107. The dimensional stability requirements placed on the membranes during this period are discussed. Interferometric techniques that provide sufficient sensitivity for these stability measurements are described. A comparison is made between the different techniques that have been developed in term of the information that each technique provides, the accuracy of the various techniques, and the implementation issues that are involved with each technique.

Advances in functional X-ray imaging techniques and contrast agents

PubMed Central

Chen, Hongyu; Rogalski, Melissa M.

2012-01-01

X-rays have been used for non-invasive high-resolution imaging of thick biological specimens since their discovery in 1895. They are widely used for structural imaging of bone, metal implants, and cavities in soft tissue. Recently, a number of new contrast methodologies have emerged which are expanding X-ray’s biomedical applications to functional as well as structural imaging. These techniques are promising to dramatically improve our ability to study in situ biochemistry and disease pathology. In this review, we discuss how X-ray absorption, X-ray fluorescence, and X-ray excited optical luminescence can be used for physiological, elemental, and molecular imaging of vasculature, tumours, pharmaceutical distribution, and the surface of implants. Imaging of endogenous elements, exogenous labels, and analytes detected with optical indicators will be discussed. PMID:22962667

Determining the Uncertainty of X-Ray Absorption Measurements

PubMed Central

Wojcik, Gary S.

2004-01-01

X-ray absorption (or more properly, x-ray attenuation) techniques have been applied to study the moisture movement in and moisture content of materials like cement paste, mortar, and wood. An increase in the number of x-ray counts with time at a location in a specimen may indicate a decrease in moisture content. The uncertainty of measurements from an x-ray absorption system, which must be known to properly interpret the data, is often assumed to be the square root of the number of counts, as in a Poisson process. No detailed studies have heretofore been conducted to determine the uncertainty of x-ray absorption measurements or the effect of averaging data on the uncertainty. In this study, the Poisson estimate was found to adequately approximate normalized root mean square errors (a measure of uncertainty) of counts for point measurements and profile measurements of water specimens. The Poisson estimate, however, was not reliable in approximating the magnitude of the uncertainty when averaging data from paste and mortar specimens. Changes in uncertainty from differing averaging procedures were well-approximated by a Poisson process. The normalized root mean square errors decreased when the x-ray source intensity, integration time, collimator size, and number of scanning repetitions increased. Uncertainties in mean paste and mortar count profiles were kept below 2 % by averaging vertical profiles at horizontal spacings of 1 mm or larger with counts per point above 4000. Maximum normalized root mean square errors did not exceed 10 % in any of the tests conducted. PMID:27366627

X-ray absorption spectroscopic studies of mononuclear non-heme iron enzymes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Westre, Tami E.

Fe-K-edge X-ray absorption spectroscopy (XAS) has been used to investigate the electronic and geometric structure of the iron active site in non-heme iron enzymes. A new theoretical extended X-ray absorption fine structure (EXAFS) analysis approach, called GNXAS, has been tested on data for iron model complexes to evaluate the utility and reliability of this new technique, especially with respect to the effects of multiple-scattering. In addition, a detailed analysis of the 1s→3d pre-edge feature has been developed as a tool for investigating the oxidation state, spin state, and geometry of iron sites. Edge and EXAFS analyses have then been appliedmore » to the study of non-heme iron enzyme active sites.« less

X-ray absorption spectroscopy and neutron diffraction study of the perovskite-type rare-earth cobaltites

NASA Astrophysics Data System (ADS)

Sikolenko, V.; Efimova, E.; Franz, A.; Ritter, C.; Troyanchuk, I. O.; Karpinsky, D.; Zubavichus, Y.; Veligzhanin, A.; Tiutiunnikov, S. I.; Sazonov, A.; Efimov, V.

2018-05-01

Correlations between local and long-range structure distortions in the perovskite-type RE1-xSrxCoO3-δ (RE = La, Pr, Nd; x = 0.0 and 0.5) compounds have been studied at room temperature by extended X-ray absorption fine structure (EXAFS) at the Co K-edge and high-resolution neutron powder diffraction (NPD). The use of two complementary experimental techniques allowed us to explore the influence of the type of rare-earth element and strontium substitution on unusual behavior of static and dynamic features of both the Co-O bond lengths.

Determination of total x-ray absorption coefficient using non-resonant x-ray emission

PubMed Central

Achkar, A. J.; Regier, T. Z.; Monkman, E. J.; Shen, K. M.; Hawthorn, D. G.

2011-01-01

An alternative measure of x-ray absorption spectroscopy (XAS) called inverse partial fluorescence yield (IPFY) has recently been developed that is both bulk sensitive and free of saturation effects. Here we show that the angle dependence of IPFY can provide a measure directly proportional to the total x-ray absorption coefficient, µ(E). In contrast, fluorescence yield (FY) and electron yield (EY) spectra are offset and/or distorted from µ(E) by an unknown and difficult to measure amount. Moreover, our measurement can determine µ(E) in absolute units with no free parameters by scaling to µ(E) at the non-resonant emission energy. We demonstrate this technique with measurements on NiO and NdGaO3. Determining µ(E) across edge-steps enables the use of XAS as a non-destructive measure of material composition. In NdGaO3, we also demonstrate the utility of IPFY for insulating samples, where neither EY or FY provide reliable spectra due to sample charging and self-absorption effects, respectively. PMID:22355697

Application of several physical techniques in the total analysis of a canine urinary calculus.

PubMed

Rodgers, A L; Mezzabotta, M; Mulder, K J; Nassimbeni, L R

1981-06-01

A single calculus from the bladder of a Beagle bitch has been analyzed by a multiple technique approach employing x-ray diffraction, infrared spectroscopy, scanning electron microscopy, x-ray fluorescence spectrometry, atomic absorption spectrophotometry and density gradient fractionation. The qualitative and quantitative data obtained showed excellent agreement, lending confidence to such an approach for the evaluation and understanding of stone disease.

Simulations of multi-contrast x-ray imaging using near-field speckles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zdora, Marie-Christine; Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire, OX11 0DE, United Kingdom and Department of Physics & Astronomy, University College London, London, WC1E 6BT; Thibault, Pierre

2016-01-28

X-ray dark-field and phase-contrast imaging using near-field speckles is a novel technique that overcomes limitations inherent in conventional absorption x-ray imaging, i.e. poor contrast for features with similar density. Speckle-based imaging yields a wealth of information with a simple setup tolerant to polychromatic and divergent beams, and simple data acquisition and analysis procedures. Here, we present a simulation software used to model the image formation with the speckle-based technique, and we compare simulated results on a phantom sample with experimental synchrotron data. Thorough simulation of a speckle-based imaging experiment will help for better understanding and optimising the technique itself.

Establishing nonlinearity thresholds with ultraintense X-ray pulses

NASA Astrophysics Data System (ADS)

Szlachetko, Jakub; Hoszowska, Joanna; Dousse, Jean-Claude; Nachtegaal, Maarten; Błachucki, Wojciech; Kayser, Yves; Sà, Jacinto; Messerschmidt, Marc; Boutet, Sebastien; Williams, Garth J.; David, Christian; Smolentsev, Grigory; van Bokhoven, Jeroen A.; Patterson, Bruce D.; Penfold, Thomas J.; Knopp, Gregor; Pajek, Marek; Abela, Rafael; Milne, Christopher J.

2016-09-01

X-ray techniques have evolved over decades to become highly refined tools for a broad range of investigations. Importantly, these approaches rely on X-ray measurements that depend linearly on the number of incident X-ray photons. The advent of X-ray free electron lasers (XFELs) is opening the ability to reach extremely high photon numbers within ultrashort X-ray pulse durations and is leading to a paradigm shift in our ability to explore nonlinear X-ray signals. However, the enormous increase in X-ray peak power is a double-edged sword with new and exciting methods being developed but at the same time well-established techniques proving unreliable. Consequently, accurate knowledge about the threshold for nonlinear X-ray signals is essential. Herein we report an X-ray spectroscopic study that reveals important details on the thresholds for nonlinear X-ray interactions. By varying both the incident X-ray intensity and photon energy, we establish the regimes at which the simplest nonlinear process, two-photon X-ray absorption (TPA), can be observed. From these measurements we can extract the probability of this process as a function of photon energy and confirm both the nature and sub-femtosecond lifetime of the virtual intermediate electronic state.

Spectroscopic imaging, diffraction, and holography with x-ray photoemission

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1992-02-01

X-ray probes are capable of determining the spatial structure of an atom in a specific chemical state, over length scales from about a micron all the way down to atomic resolution. Examples of these probes include photoemission microscopy, energy-dependent photoemission diffraction, photoelectron holography, and X-ray absorption microspectroscopy. Although the method of image formation, chemical-state sensitivity, and length scales can be very different, these X-ray techniques share a common goal of combining a capability for structure determination with chemical-state specificity. This workshop will address recent advances in holographic, diffraction, and direct imaging techniques using X-ray photoemission on both theoretical and experimentalmore » fronts. A particular emphasis will be on novel structure determinations with atomic resolution using photoelectrons.« less

Imaging at an x-ray absorption edge using free electron laser pulses for interface dynamics in high energy density systems [Resonant phase contrast imaging for interface physics

DOE PAGES

Beckwith, M. A.; Jiang, S.; Schropp, A.; ...

2017-05-01

Tuning the energy of an x-ray probe to an absorption line or edge can provide material-specific measurements that are particularly useful for interfaces. Simulated hard x-ray images above the Fe K-edge are presented to examine ion diffusion across an interface between Fe 2O 3 and SiO 2 aerogel foam materials. The simulations demonstrate the feasibility of such a technique for measurements of density scale lengths near the interface with submicron spatial resolution. A proof-of-principle experiment is designed and performed at the Linac coherent light source facility. Preliminary data show the change of the interface after shock compression and heating withmore » simultaneous fluorescence spectra for temperature determination. Here, the results provide the first demonstration of using x-ray imaging at an absorption edge as a diagnostic to detect ultrafast phenomena for interface physics in high-energy-density systems.« less

X-ray absorption and Mössbauer spectroscopies characterization of iron nanoclusters prepared by the gas aggregation technique.

PubMed

Sánchez-Marcos, J; Laguna-Marco, M A; Martínez-Morillas, R; Céspedes, E; Menéndez, N; Jiménez-Villacorta, F; Prieto, C

2012-11-01

Partially oxidized iron nanoclusters have been prepared by the gas-phase aggregation technique with typical sizes of 2-3 nm. This preparation technique has been reported to obtain clusters with interesting magnetic properties such as very large exchange bias. In this paper, a sample composition study carried out by Mössbauer and X-ray absorption spectroscopies is reported. The information reached by these techniques, which is based on the iron short range order, results to be an ideal way to have a characterization of the whole sample since the obtained data are an average over a very large amount of the clusters. In addition, our results indicate the presence of ferrihydrite, which is a compound typically ignored when studying this type of systems.

Synchrotron X-ray studies of the keel of the short-spined sea urchin Lytechinus variegatus: absorption microtomography (microCT) and small beam diffraction mapping.

PubMed

Stock, S R; Barss, J; Dahl, T; Veis, A; Almer, J D; Carlo, F

2003-05-01

In sea urchin teeth, the keel plays an important structural role, and this paper reports results of microstructural characterization of the keel of Lytechinus variegatus using two noninvasive synchrotron x-ray techniques: x-ray absorption microtomography (microCT) and x-ray diffraction mapping. MicroCT with 14 keV x-rays mapped the spatial distribution of mineral at the 1.3 microm level in a millimeter-sized fragment of a mature portion of the keel. Two rows of low absorption channels (i.e., primary channels) slightly less than 10 microm in diameter were found running linearly from the flange to the base of the keel and parallel to its sides. The primary channels paralleled the oral edge of the keel, and the microCT slices revealed a planar secondary channel leading from each primary channel to the side of the keel. The primary and secondary channels were more or less coplanar and may correspond to the soft tissue between plates of the carinar process. Transmission x-ray diffraction with 80.8 keV x-rays and a 0.1 mm beam mapped the distribution of calcite crystal orientations and the composition Ca(1-x)Mg(x)CO(3) of the calcite. Unlike the variable Mg concentration and highly curved prisms found in the keel of Paracentrotus lividus, a constant Mg content (x = 0.13) and relatively little prism curvature was found in the keel of Lytechinus variegatus.

Applications of “Tender” Energy (1-5 keV) X-ray Absorption Spectroscopy in Life Sciences

DOE Office of Scientific and Technical Information (OSTI.GOV)

Northrup, Paul; Leri, Alessandra; Tappero, Ryan

The “tender” energy range of 1 to 5 keV, between the energy ranges of most “hard” (>5 keV) and “soft” (<1 keV) synchrotron X-ray facilities, offers some unique opportunities for synchrotron-based X-ray absorption fine structure spectroscopy in life sciences. In particular the K absorption edges of Na through Ca offer opportunities to study local structure, speciation, and chemistry of many important biological compounds, structures and processes. This is an area of largely untapped science, in part due to a scarcity of optimized facilities. Such measurements also entail unique experimental challenges. Lastly, this brief review describes the technique, its experimental challenges,more » recent progress in development of microbeam measurement capabilities, and several highlights illustrating applications in life sciences.« less

Determination of K shell absorption jump factors and jump ratios of 3d transition metals by measuring K shell fluorescence parameters.

PubMed

Kaçal, Mustafa Recep; Han, İbrahim; Akman, Ferdi

2015-01-01

Energy dispersive X-ray fluorescence technique (EDXRF) has been employed for measuring K-shell absorption jump factors and jump ratios for Ti, Cr, Fe, Co, Ni and Cu elements. The jump factors and jump ratios for these elements were determined by measuring K shell fluorescence parameters such as the Kα X-ray production cross-sections, K shell fluorescence yields, Kβ-to-Kα X-rays intensity ratios, total atomic absorption cross sections and mass attenuation coefficients. The measurements were performed using a Cd-109 radioactive point source and an Si(Li) detector in direct excitation and transmission experimental geometry. The measured values for jump factors and jump ratios were compared with theoretically calculated and the ones available in the literature. Copyright © 2014 Elsevier Ltd. All rights reserved.

Applications of “Tender” Energy (1-5 keV) X-ray Absorption Spectroscopy in Life Sciences

DOE PAGES

Northrup, Paul; Leri, Alessandra; Tappero, Ryan

2016-02-15

The “tender” energy range of 1 to 5 keV, between the energy ranges of most “hard” (>5 keV) and “soft” (<1 keV) synchrotron X-ray facilities, offers some unique opportunities for synchrotron-based X-ray absorption fine structure spectroscopy in life sciences. In particular the K absorption edges of Na through Ca offer opportunities to study local structure, speciation, and chemistry of many important biological compounds, structures and processes. This is an area of largely untapped science, in part due to a scarcity of optimized facilities. Such measurements also entail unique experimental challenges. Lastly, this brief review describes the technique, its experimental challenges,more » recent progress in development of microbeam measurement capabilities, and several highlights illustrating applications in life sciences.« less

Structural and optical properties of furfurylidenemalononitrile thin films

NASA Astrophysics Data System (ADS)

Ali, H. A. M.

2013-03-01

Thin films of furfurylidenemalononitrile (FMN) were deposited on different substrates at room temperature by thermal evaporation technique under a high vacuum. The structure of the powder was confirmed by Fourier transformation infrared (FTIR) technique. The unit cell dimensions were determined from X-ray diffraction (XRD) studies. The optical properties were investigated using spectrophotometric measurements of the transmittance and reflectance at normal incidence of light in the wavelength range from 200 to 2500 nm. The refractive index (n), the absorption index (k) and the absorption coefficient (α) were calculated. The analysis of the spectral behavior of the absorption coefficient in the absorption region revealed an indirect allowed transition. The refractive index dispersion was analyzed using the single oscillator model. Some dispersion parameters were estimated. Complex dielectric function and optical conductivity were determined. The influence of the irradiation with high-energy X-rays (6 MeV) on the studied properties was also investigated.

Masked-backlighter technique used to simultaneously image x-ray absorption and x-ray emission from an inertial confinement fusion plasma.

PubMed

Marshall, F J; Radha, P B

2014-11-01

A method to simultaneously image both the absorption and the self-emission of an imploding inertial confinement fusion plasma has been demonstrated on the OMEGA Laser System. The technique involves the use of a high-Z backlighter, half of which is covered with a low-Z material, and a high-speed x-ray framing camera aligned to capture images backlit by this masked backlighter. Two strips of the four-strip framing camera record images backlit by the high-Z portion of the backlighter, while the other two strips record images aligned with the low-Z portion of the backlighter. The emission from the low-Z material is effectively eliminated by a high-Z filter positioned in front of the framing camera, limiting the detected backlighter emission to that of the principal emission line of the high-Z material. As a result, half of the images are of self-emission from the plasma and the other half are of self-emission plus the backlighter. The advantage of this technique is that the self-emission simultaneous with backlighter absorption is independently measured from a nearby direction. The absorption occurs only in the high-Z backlit frames and is either spatially separated from the emission or the self-emission is suppressed by filtering, or by using a backlighter much brighter than the self-emission, or by subtraction. The masked-backlighter technique has been used on the OMEGA Laser System to simultaneously measure the emission profiles and the absorption profiles of polar-driven implosions.

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

Time Resolved X-Ray Spectral Analysis of Class II YSOs in NGC 2264 During Optical Dips and Bursts

NASA Astrophysics Data System (ADS)

Guarcello, Mario Giuseppe; Flaccomio, Ettore; Micela, Giuseppina; Argiroffi, Costanza; Venuti, Laura

2016-07-01

Pre-Main Sequence stars are variable sources. The main mechanisms responsible for their variability are variable extinction, unsteady accretion, and rotational modulation of both hot and dark photospheric spots and X-ray active regions. In stars with disks this variability is thus related to the morphology of the inner circumstellar region (<0.1 AU) and that of photosphere and corona, all impossible to be spatially resolved with present day techniques. This has been the main motivations of the Coordinated Synoptic Investigation of NGC2264, a set of simultaneous observations of NGC2264 with 15 different telescopes.We analyze the X-ray spectral properties of stars with disks extracted during optical bursts and dips in order to unveil the nature of these phenomena. Stars are analyzed in two different samples. In stars with variable extinction a simultaneous increase of optical extinction and X-ray absorption is searched during the optical dips; in stars with accretion bursts we search for soft X-ray emission and increasing X-ray absorption during the bursts. In 9/33 stars with variable extinction we observe simultaneous increase of X-ray absorption and optical extinction. In seven dips it is possible to calculate the NH/AV ratio in order to infer the composition of the obscuring material. In 5/27 stars with optical accretion bursts, we observe soft X-ray emission during the bursts that we associate to the emission of accreting gas. It is not surprising that these properties are not observed in all the stars with dips and bursts since favorable geometric configurations are required. The observed variable absorption during the dips is mainly due to dust-free material in accretion streams. In stars with accretion bursts we observe in average a larger soft X-ray spectral component not observed in non accreting stars. This indicates that this soft X-ray emission arises from the accretion shocks.

Soft X-ray spectroscopy of nanoparticles by velocity map imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kostko, O.; Xu, B.; Jacobs, M. I.

Velocity map imaging (VMI), a technique traditionally used to study chemical dynamics in the gas phase, is applied to study X-ray photoemission from aerosol nanoparticles. Soft X-rays from the Advanced Light Source synchrotron, probe a beam of nanoparticles, and the resulting photoelectrons are velocity mapped to obtain their kinetic energy distributions. A new design of the VMI spectrometer is described. The spectrometer is benchmarked by measuring vacuum ultraviolet photoemission from gas phase xenon and squalene nanoparticles followed by measurements using soft X-rays. It is demonstrated that the photoelectron distribution from X-ray irradiated squalene nanoparticles is dominated by secondary electrons. Bymore » scanning the photon energies and measuring the intensities of these secondary electrons, a near edge X-ray absorption fine structure (NEXAFS) spectrum is obtained. The NEXAFS technique is used to obtain spectra of aqueous nanoparticles at the oxygen K edge. By varying the position of the aqueous nanoparticle beam relative to the incident X-ray beam, evidence is presented such that the VMI technique allows for NEXAFS spectroscopy of water in different physical states. Finally, we discuss the possibility of applying VMI methods to probe liquids and solids via X-ray spectroscopy.« less

Soft X-ray spectroscopy of nanoparticles by velocity map imaging

DOE PAGES

Kostko, O.; Xu, B.; Jacobs, M. I.; ...

2017-05-05

Velocity map imaging (VMI), a technique traditionally used to study chemical dynamics in the gas phase, is applied to study X-ray photoemission from aerosol nanoparticles. Soft X-rays from the Advanced Light Source synchrotron, probe a beam of nanoparticles, and the resulting photoelectrons are velocity mapped to obtain their kinetic energy distributions. A new design of the VMI spectrometer is described. The spectrometer is benchmarked by measuring vacuum ultraviolet photoemission from gas phase xenon and squalene nanoparticles followed by measurements using soft X-rays. It is demonstrated that the photoelectron distribution from X-ray irradiated squalene nanoparticles is dominated by secondary electrons. Bymore » scanning the photon energies and measuring the intensities of these secondary electrons, a near edge X-ray absorption fine structure (NEXAFS) spectrum is obtained. The NEXAFS technique is used to obtain spectra of aqueous nanoparticles at the oxygen K edge. By varying the position of the aqueous nanoparticle beam relative to the incident X-ray beam, evidence is presented such that the VMI technique allows for NEXAFS spectroscopy of water in different physical states. Finally, we discuss the possibility of applying VMI methods to probe liquids and solids via X-ray spectroscopy.« less

Development of an X-ray prism for a combined diffraction enhanced imaging and fluorescence imaging system

NASA Astrophysics Data System (ADS)

Bewer, Brian E.

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These X-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing a large change in intensity for a small angle change introduced by the X-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultra small angle X-ray scattering (USAXS) contrast thus improving visualization and extending the utility of X-ray imaging. To improve on the current DEI technique this body of work describes the design of an X-ray prism (XRP) included in the imaging system which allows the analyzer crystal to be aligned anywhere on the rocking curve without moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from muradians for direct mechanical movement of the analyzer crystal to milliradian control for movement the XRP angle. In addition to using an XRP for the traditional DEI acquisition method of two scans on opposite sides of the rocking curve preliminary tests will be presented showing the potential of using an XRP to scan quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single fast measurement thus removing the occurrence of motion artifacts for each point or line used during a scan. The XRP design is also intended to be compatible with combined imaging systems where more than one technique is used to investigate a sample. Candidates for complimentary techniques are investigated and measurements from a combined X-ray imaging system are presented.

X-ray absorption spectroscopic studies on gold nanoparticles in mesoporous and microporous materials.

PubMed

Akolekar, Deepak B; Foran, Garry; Bhargava, Suresh K

2004-05-01

Au L(3)-edge X-ray absorption spectroscopic measurements were carried out over a series of mesoporous and microporous materials containing gold nanoparticles to investigate the effects of the host matrix and preparation methods on the properties of gold nanoparticles. The materials of structure type MCM-41, ZSM-5, SAPO-18 and LSX with varying framework composition containing low concentrations of gold nanoparticles were prepared and characterized. In these materials the size of the gold nanoparticles varied in the range approximately 1 to 4 nm. A series of gold nanoparticles within different mesoporous and microporous materials have been investigated using X-ray absorption fine structure (XANES, EXAFS) and other techniques. Information such as atomic distances, bonding and neighbouring environment obtained from XAFS measurements was useful in elucidating the nature and structure of gold nanoparticles on these catalytic materials. The influence of the high-temperature (823, 1113, 1273 K) treatment on gold nanoparticles inside the mesoporous matrix was investigated using the XAFS technique. The XAFS and XANES results confirm various characteristics of gold nanoparticles in these materials suitable for catalysis, fabrication of nanodevices and other applications.

Influence of oxygen on growth of carbon thin films

NASA Astrophysics Data System (ADS)

Kumar, Prabhat; Gupta, Mukul; Phase, D. M.; Stahn, Jochen

2018-04-01

In this work we studied the influence of oxygen gas on growth of carbon thin films in a magnetron sputtering process. X-ray absorption spectroscopy (XAS), x-ray and neutron reflectivity techniques were used to probe carbon thin films deposited with and without oxygen at room temperature. XAS in particularly x-ray absorption near edge spectroscopy (XANES) is powerful technique to identify the nature of hybridization of carbon atoms with other elements. In a XANES pattern, presence of C=O and C-O bonds is generally observed in spite of the fact that oxygen has not been deliberately included in the growth process. In order to confirm the presence of such features, we introduced a small amount of oxygen at 1% during the growth of carbon thin films. Though such additions do not affect the number density as observed by x-ray and neutron reflectivity, they severally affect the C K-edge spectra as evidenced by an enhancement in carbon-oxygen hybridization. Observed results are helpful in analyzing the C K-edge spectra more confidently.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review.

PubMed

Dwivedi, D; Lepkova, K; Becker, T

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

NASA Astrophysics Data System (ADS)

Dwivedi, D.; Lepkova, K.; Becker, T.

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

PubMed Central

Dwivedi, D.; Becker, T.

2017-01-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed. PMID:28413351

Pump-Flow-Probe X-Ray Absorption Spectroscopy as a Tool for Studying Intermediate States of Photocatalytic Systems.

PubMed

Smolentsev, Grigory; Guda, Alexander; Zhang, Xiaoyi; Haldrup, Kristoffer; Andreiadis, Eugen; Chavarot-Kerlidou, Murielle; Canton, Sophie E; Nachtegaal, Maarten; Artero, Vincent; Sundstrom, Villy

2013-08-29

A new setup for pump-flow-probe X-ray absorption spectroscopy has been implemented at the SuperXAS beamline of the Swiss Light Source. It allows recording X-ray absorption spectra with a time resolution of tens of microseconds and high detection efficiency for samples with sub-mM concentrations. A continuous wave laser is used for the photoexcitation, with the distance between laser and X-ray beams and velocity of liquid flow determining the time delay, while the focusing of both beams and the flow speed define the time resolution. This method is compared with the alternative measurement technique that utilizes a 1 kHz repetition rate laser and multiple X-ray probe pulses. Such an experiment was performed at beamline 11ID-D of the Advanced Photon Source. Advantages, limitations and potential for improvement of the pump-flow-probe setup are discussed by analyzing the photon statistics. Both methods, with Co K-edge probing were applied to the investigation of a cobaloxime-based photo-catalytic reaction. The interplay between optimizing for efficient photoexcitation and time resolution as well as the effect of sample degradation for these two setups are discussed.

Pump-Flow-Probe X-Ray Absorption Spectroscopy as a Tool for Studying Intermediate States of Photocatalytic Systems

PubMed Central

Smolentsev, Grigory; Guda, Alexander; Zhang, XIaoyi; Haldrup, Kristoffer; Andreiadis, Eugen; Chavarot-Kerlidou, Murielle; Canton, Sophie E.; Nachtegaal, Maarten; Artero, Vincent; Sundstrom, Villy

2014-01-01

A new setup for pump-flow-probe X-ray absorption spectroscopy has been implemented at the SuperXAS beamline of the Swiss Light Source. It allows recording X-ray absorption spectra with a time resolution of tens of microseconds and high detection efficiency for samples with sub-mM concentrations. A continuous wave laser is used for the photoexcitation, with the distance between laser and X-ray beams and velocity of liquid flow determining the time delay, while the focusing of both beams and the flow speed define the time resolution. This method is compared with the alternative measurement technique that utilizes a 1 kHz repetition rate laser and multiple X-ray probe pulses. Such an experiment was performed at beamline 11ID-D of the Advanced Photon Source. Advantages, limitations and potential for improvement of the pump-flow-probe setup are discussed by analyzing the photon statistics. Both methods, with Co K-edge probing were applied to the investigation of a cobaloxime-based photo-catalytic reaction. The interplay between optimizing for efficient photoexcitation and time resolution as well as the effect of sample degradation for these two setups are discussed. PMID:24443663

Investigating the Defect Structures in Transparent Conducting Oxides Using X-ray and Neutron Scattering Techniques

PubMed Central

González, Gabriela B.

2012-01-01

Transparent conducting oxide (TCO) materials are implemented into a wide variety of commercial devices because they possess a unique combination of high optical transparency and high electrical conductivity. Created during the processing of the TCOs, defects within the atomic-scale structure are responsible for their desirable optical and electrical properties. Therefore, studying the defect structure is essential to a better understanding of the behavior of transparent conductors. X-ray and neutron scattering techniques are powerful tools to investigate the atomic lattice structural defects in these materials. This review paper presents some of the current developments in the study of structural defects in n-type TCOs using x-ray diffraction (XRD), neutron diffraction, extended x-ray absorption fine structure (EXAFS), pair distribution functions (PDFs), and x-ray fluorescence (XRF). PMID:28817010

Measurement techniques for trace metals in coal-plant effluents: A brief review

NASA Technical Reports Server (NTRS)

Singh, J. J.

1979-01-01

The strong features and limitations of techniques for determining trace elements in aerosols emitted from coal plants are discussed. Techniques reviewed include atomic absorption spectroscopy, charged particle scattering and activation, instrumental neutron activation analysis, gas/liquid chromatography, gas chromatographic/mass spectrometric methods, X-ray fluorescence, and charged-particle-induced X-ray emission. The latter two methods are emphasized. They provide simultaneous, sensitive multielement analyses and lend themselves readily to depth profiling. It is recommended that whenever feasible, two or more complementary techniques should be used for analyzing environmental samples.

Morphology, stability, and X-ray absorption spectroscopic study of iron oxide (Hematite) nanoparticles prepared by micelle nanolithography

NASA Astrophysics Data System (ADS)

Bera, Anupam; Bhattacharya, Atanu; Tiwari, N.; Jha, S. N.; Bhattacharyya, D.

2018-03-01

Currently, considerable effort is being made towards synthesis and characterization of iron oxide nanoparticles. In this article, we report on the preparation and characterization of iron oxide nanoparticle (NP) arrays supported on natively oxidized Si(100) surface. The NPs are synthesized by reverse micelle nanolithography technique and are then deposited onto natively oxidized Si(100) surface via spin-coating. Plasma oxidation followed by high temperature annealing results in a unimodal size distribution of pseudohexagonally-ordered array of iron oxide NPs (with ∼14 nm mean diameter and ∼5 nm mean height). High temperature annealing does not fragment the NPs. Particles are sinter-resistant: the unimodal arrays are robust with respect to thermal treatment. X-ray absorption spectroscopy (XAS), including X-ray Absorption Near Edge Structure (XANES) and Extended X-ray Absorption Fine Structure (EXAFS), reveals that structure of the iron oxide particle resembles closely the hematite α-Fe2O3 structure. Furthermore, with the help of EXAFS spectra, we eliminate the possibility of γ-Fe2O3, Fe3O4, FeO and FeO(OH) structures for the NPs.

Establishing nonlinearity thresholds with ultraintense X-ray pulses

DOE PAGES

Szlachetko, Jakub; Hoszowska, Joanna; Dousse, Jean-Claude; ...

2016-09-13

X-ray techniques have evolved over decades to become highly refined tools for a broad range of investigations. Importantly, these approaches rely on X-ray measurements that depend linearly on the number of incident X-ray photons. The advent of X-ray free electron lasers (XFELs) is opening the ability to reach extremely high photon numbers within ultrashort X-ray pulse durations and is leading to a paradigm shift in our ability to explore nonlinear X-ray signals. However, the enormous increase in X-ray peak power is a double-edged sword with new and exciting methods being developed but at the same time well-established techniques proving unreliable.more » Consequently, accurate knowledge about the threshold for nonlinear X-ray signals is essential. Here in this paper we report an X-ray spectroscopic study that reveals important details on the thresholds for nonlinear X-ray interactions. By varying both the incident X-ray intensity and photon energy, we establish the regimes at which the simplest nonlinear process, two-photon X-ray absorption (TPA), can be observed. From these measurements we can extract the probability of this process as a function of photon energy and confirm both the nature and sub-femtosecond lifetime of the virtual intermediate electronic state.« less

Elemental-sensitive Detection of the Chemistry in Batteries through Soft X-ray Absorption Spectroscopy and Resonant Inelastic X-ray Scattering.

PubMed

Wu, Jinpeng; Sallis, Shawn; Qiao, Ruimin; Li, Qinghao; Zhuo, Zengqing; Dai, Kehua; Guo, Zixuan; Yang, Wanli

2018-04-17

Energy storage has become more and more a limiting factor of today's sustainable energy applications, including electric vehicles and green electric grid based on volatile solar and wind sources. The pressing demand of developing high-performance electrochemical energy storage solutions, i.e., batteries, relies on both fundamental understanding and practical developments from both the academy and industry. The formidable challenge of developing successful battery technology stems from the different requirements for different energy-storage applications. Energy density, power, stability, safety, and cost parameters all have to be balanced in batteries to meet the requirements of different applications. Therefore, multiple battery technologies based on different materials and mechanisms need to be developed and optimized. Incisive tools that could directly probe the chemical reactions in various battery materials are becoming critical to advance the field beyond its conventional trial-and-error approach. Here, we present detailed protocols for soft X-ray absorption spectroscopy (sXAS), soft X-ray emission spectroscopy (sXES), and resonant inelastic X-ray scattering (RIXS) experiments, which are inherently elemental-sensitive probes of the transition-metal 3d and anion 2p states in battery compounds. We provide the details on the experimental techniques and demonstrations revealing the key chemical states in battery materials through these soft X-ray spectroscopy techniques.

Hyper-filter-fluorescer spectrometer for x-rays above 120 keV

DOEpatents

Wang, Ching L.

1983-01-01

An apparatus utilizing filter-fluorescer combinations is provided to measure short bursts of high fluence x-rays above 120 keV energy, where there are no practical absorption edges available for conventional filter-fluorescer techniques. The absorption edge of the prefilter is chosen to be less than that of the fluorescer, i.e., E.sub.PRF E.sub.F. In this way, the response function is virtually zero between E.sub.PRF and E.sub.F and well defined and enhanced in an energy band of less than 1000 keV above the 120 keV energy.

MICROANALYSIS OF MATERIALS USING SYNCHROTRON RADIATION.

DOE Office of Scientific and Technical Information (OSTI.GOV)

JONES,K.W.; FENG,H.

2000-12-01

High intensity synchrotron radiation produces photons with wavelengths that extend from the infrared to hard x rays with energies of hundreds of keV with uniquely high photon intensities that can be used to determine the composition and properties of materials using a variety of techniques. Most of these techniques represent extensions of earlier work performed with ordinary tube-type x-ray sources. The properties of the synchrotron source such as the continuous range of energy, high degree of photon polarization, pulsed beams, and photon flux many orders of magnitude higher than from x-ray tubes have made possible major advances in the possiblemore » chemical applications. We describe here ways that materials analyses can be made using the high intensity beams for measurements with small beam sizes and/or high detection sensitivity. The relevant characteristics of synchrotron x-ray sources are briefly summarized to give an idea of the x-ray parameters to be exploited. The experimental techniques considered include x-ray fluorescence, absorption, and diffraction. Examples of typical experimental apparatus used in these experiments are considered together with descriptions of actual applications.« less

Identifying anthropogenic uranium compounds using soft X-ray near-edge absorption spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ward, Jesse D.; Bowden, Mark; Tom Resch, C.

2017-01-01

Uranium ores mined for industrial use are typically acid-leached to produce yellowcake and then converted into uranium halides for enrichment and purification. These anthropogenic chemical forms of uranium are distinct from their mineral counterparts. The purpose of this study is to use soft X-ray absorption spectroscopy to characterize several common anthropogenic uranium compounds important to the nuclear fuel cycle. Non-destructive chemical analyses of these compounds is important for process and environmental monitoring and X-ray absorption techniques have several advantages in this regard, including element-specificity, chemical sensitivity, and high spectral resolution. Oxygen K-edge spectra were collected for uranyl nitrate, uranyl fluoride,more » and uranyl chloride, and fluorine K-edge spectra were collected for uranyl fluoride and uranium tetrafluoride. Interpretation of the data is aided by comparisons to calculated spectra. These compounds have unique spectral signatures that can be used to identify unknown samples.« less

X-ray spatial frequency heterodyne imaging of protein-based nanobubble contrast agents

PubMed Central

Rand, Danielle; Uchida, Masaki; Douglas, Trevor; Rose-Petruck, Christoph

2014-01-01

Spatial Frequency Heterodyne Imaging (SFHI) is a novel x-ray scatter imaging technique that utilizes nanoparticle contrast agents. The enhanced sensitivity of this new technique relative to traditional absorption-based x-ray radiography makes it promising for applications in biomedical and materials imaging. Although previous studies on SFHI have utilized only metal nanoparticle contrast agents, we show that nanomaterials with a much lower electron density are also suitable. We prepared protein-based “nanobubble” contrast agents that are comprised of protein cage architectures filled with gas. Results show that these nanobubbles provide contrast in SFHI comparable to that of gold nanoparticles of similar size. PMID:25321797

Feasibility of Valence-to-Core X-ray Emission Spectroscopy for Tracking Transient Species

DOE PAGES

March, Anne Marie; Assefa, Tadesse A.; Bressler, Christian; ...

2015-02-09

X-ray spectroscopies, when combined in laser-pump, X-ray-probe measurement schemes, can be powerful tools for tracking the electronic and geometric structural changes that occur during the course of a photoinitiated chemical reaction. X-ray absorption spectroscopy (XAS) is considered an established technique for such measurements, and X-ray emission spectroscopy (XES) of the strongest core-to-core emission lines (Kα and Kβ) is now being utilized. Flux demanding valence-to-core XES promises to be an important addition to the time-resolved spectroscopic toolkit. Here In this paper we present measurements and density functional theory calculations on laser-excited, solution-phase ferrocyanide that demonstrate the feasibility of valence-to-core XES formore » time-resolved experiments. Lastly, we discuss technical improvements that will make valence-to-core XES a practical pump–probe technique.« less

Effect of iron oxide reductive dissolution on the transformation and immobilization of arsenic in soils: New insights from X-ray photoelectron and X-ray absorption spectroscopy.

PubMed

Fan, Jian-Xin; Wang, Yu-Jun; Liu, Cun; Wang, Li-Hua; Yang, Ke; Zhou, Dong-Mei; Li, Wei; Sparks, Donald L

2014-08-30

The geochemical behavior and speciation of arsenic (As) in paddy soils is strongly controlled by soil redox conditions and the sequestration by soil iron oxyhydroxides. Hence, the effects of iron oxide reductive dissolution on the adsorption, transformation and precipitation of As(III) and As(V) in soils were investigated using batch experiments and synchrotron based techniques to gain a deeper understanding at both macroscopic and microscopic scales. The results of batch sorption experiments revealed that the sorption capacity of As(V) on anoxic soil was much higher than that on control soil. Synchrotron based X-ray fluorescence (μ-XRF) mapping studies indicated that As was heterogeneously distributed and was mainly associated with iron in the soil. X-ray absorption near edge structure (XANES), micro-X-ray absorption near edge structure (μ-XANES) and X-ray photoelectron spectroscopy (XPS) analyses revealed that the primary speciation of As in the soil is As(V). These results further suggested that, when As(V) was introduced into the anoxic soil, the rapid coprecipitation of As(V) with ferric/ferrous ion prevented its reduction to As(III), and was the main mechanism controlling the immobilization of As. This research could improve the current understanding of soil As chemistry in paddy and wetland soils. Copyright © 2014 Elsevier B.V. All rights reserved.

LabVIEW interface with Tango control system for a multi-technique X-ray spectrometry IAEA beamline end-station at Elettra Sincrotrone Trieste

NASA Astrophysics Data System (ADS)

Wrobel, P. M.; Bogovac, M.; Sghaier, H.; Leani, J. J.; Migliori, A.; Padilla-Alvarez, R.; Czyzycki, M.; Osan, J.; Kaiser, R. B.; Karydas, A. G.

2016-10-01

A new synchrotron beamline end-station for multipurpose X-ray spectrometry applications has been recently commissioned and it is currently accessible by end-users at the XRF beamline of Elettra Sincrotrone Trieste. The end-station consists of an ultra-high vacuum chamber that includes as main instrument a seven-axis motorized manipulator for sample and detectors positioning, different kinds of X-ray detectors and optical cameras. The beamline end-station allows performing measurements in different X-ray spectrometry techniques such as Microscopic X-Ray Fluorescence analysis (μXRF), Total Reflection X-Ray Fluorescence analysis (TXRF), Grazing Incidence/Exit X-Ray Fluorescence analysis (GI-XRF/GE-XRF), X-Ray Reflectometry (XRR), and X-Ray Absorption Spectroscopy (XAS). A LabVIEW Graphical User Interface (GUI) bound with Tango control system consisted of many custom made software modules is utilized as a user-friendly tool for control of the entire end-station hardware components. The present work describes this advanced Tango and LabVIEW software platform that utilizes in an optimal synergistic manner the merits and functionality of these well-established programming and equipment control tools.

Forcing Cesium into Higher Oxidation States Using Useful hard x-ray Induced Chemistry under High Pressure

NASA Astrophysics Data System (ADS)

Sneed, D.; Pravica, M.; Kim, E.; Chen, N.; Park, C.; White, M.

2017-10-01

This paper discusses our attempt to synthesize higher oxidation forms of cesium fluoride by pressurizing cesium fluoride in a fluorine-rich environment created via the x-ray decomposition of potassium tetrafluoroborate. This was done in order to confirm recent theoretical predictions of higher oxidation forms of CsFn. We discuss the development of a technique to produce molecular fluorine in situ via useful hard x-ray photochemistry, and the attempt to utilize this technique to form higher oxidation states of cesium fluoride. In order to verify the formation of the novel stoichiometric species of CsFn. X-ray Absorption Near Edge Spectroscopy (XANES) centered on the cesium K-edge was performed to probe the oxidation state of cesium as well as the local molecular coordination around Cs.

Effect of PbO on optical properties of tellurite glass

NASA Astrophysics Data System (ADS)

Elazoumi, S. H.; Sidek, H. A. A.; Rammah, Y. S.; El-Mallawany, R.; Halimah, M. K.; Matori, K. A.; Zaid, M. H. M.

2018-03-01

Binary (1 - x)(TeO2) - x(PbO), x = 0, 0.10, 0.15, 0.20, 0.25, 0.30 mol% glass system was fabricated using melt quenching method. X-ray diffraction (XRD) technique was employed to confirm the amorphous nature. The microanalysis of the major components was performed using energy dispersive EDX and X-ray spectrometry. Both the molar volume and the density were measured. FTIR and UV spectra were recorded at 400-4000 cm-1 and 220-800 nm, respectively. The optical band gap (Eopt), Urbach's energy (Eu), index of refraction (n) were calculated using absorption spectrum fitting (ASF) and derivation of absorption spectrum fitting (DASF) methods. Molar refraction Rm and molecular polarizability αm have been calculated according to (ASF) method.

High resolution x-ray microtomography of biological samples: Requirements and strategies for satisfying them

DOE Office of Scientific and Technical Information (OSTI.GOV)

Loo, B.W. Jr.

High resolution x-ray microscopy has been made possible in recent years primarily by two new technologies: microfabricated diffractive lenses for soft x-rays with about 30-50 nm resolution, and high brightness synchrotron x-ray sources. X-ray microscopy occupies a special niche in the array of biological microscopic imaging methods. It extends the capabilities of existing techniques mainly in two areas: a previously unachievable combination of sub-visible resolution and multi-micrometer sample size, and new contrast mechanisms. Because of the soft x-ray wavelengths used in biological imaging (about 1-4 nm), XM is intermediate in resolution between visible light and electron microscopies. Similarly, the penetrationmore » depth of soft x-rays in biological materials is such that the ideal sample thickness for XM falls in the range of 0.25 - 10 {mu}m, between that of VLM and EM. XM is therefore valuable for imaging of intermediate level ultrastructure, requiring sub-visible resolutions, in intact cells and subcellular organelles, without artifacts produced by thin sectioning. Many of the contrast producing and sample preparation techniques developed for VLM and EM also work well with XM. These include, for example, molecule specific staining by antibodies with heavy metal or fluorescent labels attached, and sectioning of both frozen and plastic embedded tissue. However, there is also a contrast mechanism unique to XM that exists naturally because a number of elemental absorption edges lie in the wavelength range used. In particular, between the oxygen and carbon absorption edges (2.3 and 4.4 nm wavelength), organic molecules absorb photons much more strongly than does water, permitting element-specific imaging of cellular structure in aqueous media, with no artifically introduced contrast agents. For three-dimensional imaging applications requiring the capabilities of XM, an obvious extension of the technique would therefore be computerized x-ray microtomography (XMT).« less

Quantitative X-ray mapping, scatter diagrams and the generation of correction maps to obtain more information about your material

NASA Astrophysics Data System (ADS)

Wuhrer, R.; Moran, K.

2014-03-01

Quantitative X-ray mapping with silicon drift detectors and multi-EDS detector systems have become an invaluable analysis technique and one of the most useful methods of X-ray microanalysis today. The time to perform an X-ray map has reduced considerably with the ability to map minor and trace elements very accurately due to the larger detector area and higher count rate detectors. Live X-ray imaging can now be performed with a significant amount of data collected in a matter of minutes. A great deal of information can be obtained from X-ray maps. This includes; elemental relationship or scatter diagram creation, elemental ratio mapping, chemical phase mapping (CPM) and quantitative X-ray maps. In obtaining quantitative x-ray maps, we are able to easily generate atomic number (Z), absorption (A), fluorescence (F), theoretical back scatter coefficient (η), and quantitative total maps from each pixel in the image. This allows us to generate an image corresponding to each factor (for each element present). These images allow the user to predict and verify where they are likely to have problems in our images, and are especially helpful to look at possible interface artefacts. The post-processing techniques to improve the quantitation of X-ray map data and the development of post processing techniques for improved characterisation are covered in this paper.

Fabrication of absorption gratings with X-ray lithography for X-ray phase contrast imaging

NASA Astrophysics Data System (ADS)

Wang, Bo; Wang, Yu-Ting; Yi, Fu-Ting; Zhang, Tian-Chong; Liu, Jing; Zhou, Yue

2018-05-01

Grating-based X-ray phase contrast imaging is promising especially in the medical area. Two or three gratings are involved in grating-based X-ray phase contrast imaging in which the absorption grating of high-aspect-ratio is the most important device and the fabrication process is a great challenge. The material with large atomic number Z is used to fabricate the absorption grating for excellent absorption of X-ray, and Au is usually used. The fabrication process, which involves X-ray lithography, development and gold electroplating, is described in this paper. The absorption gratings with 4 μm period and about 100 μm height are fabricated and the high-aspect-ratio is 50.

Understanding refraction contrast using a comparison of absorption and refraction computed tomographic techniques

NASA Astrophysics Data System (ADS)

Wiebe, S.; Rhoades, G.; Wei, Z.; Rosenberg, A.; Belev, G.; Chapman, D.

2013-05-01

Refraction x-ray contrast is an imaging modality used primarily in a research setting at synchrotron facilities, which have a biomedical imaging research program. The most common method for exploiting refraction contrast is by using a technique called Diffraction Enhanced Imaging (DEI). The DEI apparatus allows the detection of refraction between two materials and produces a unique ''edge enhanced'' contrast appearance, very different from the traditional absorption x-ray imaging used in clinical radiology. In this paper we aim to explain the features of x-ray refraction contrast as a typical clinical radiologist would understand. Then a discussion regarding what needs to be considered in the interpretation of the refraction image takes place. Finally we present a discussion about the limitations of planar refraction imaging and the potential of DEI Computed Tomography. This is an original work that has not been submitted to any other source for publication. The authors have no commercial interests or conflicts of interest to disclose.

A flexible gas flow reaction cell for in situ x-ray absorption spectroscopy studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kroner, Anna B., E-mail: anna.kroner@diamond.ac.uk; Gilbert, Martin; Duller, Graham

2016-07-27

A capillary-based sample environment with hot air blower and integrated gas system was developed at Diamond to conduct X-ray absorption spectroscopy (XAS) studies of materials under time-resolved, in situ conditions. The use of a hot air blower, operating in the temperature range of 298-1173 K, allows introduction of other techniques e.g. X-ray diffraction (XRD), Raman spectroscopy for combined techniques studies. The flexibility to use either quartz or Kapton capillaries allows users to perform XAS measurement at energies as low as 5600 eV. To demonstrate performance, time-resolved, in situ XAS results of Rh catalysts during the process of activation (Rh K-edge,more » Ce L{sub 3}-edge and Cr K-edge) and the study of mixed oxide membrane (La{sub 0.6}Sr{sub 0.4}Co{sub 0.2}Fe{sub 0.8}O{sub 3−δ}) under various partial oxygen pressure conditions are described.« less

Studies on absorption coefficient near edge of multi elements

NASA Astrophysics Data System (ADS)

Eisa, M. H.; Shen, H.; Yao, H. Y.; Mi, Y.; Zhou, Z. Y.; Hu, T. D.; Xie, Y. N.

2005-12-01

X-ray absorption near edge structure (XANES) was used to study the near edge mass-absorption coefficients of seven elements, such as, Ti, V, Fe, Co, Ni, Cu and Zn. It is well known that, on the near edge absorption of element, when incident X-ray a few eV change can make the absorption coefficient an order magnitude alteration. So that, there are only a few points mass-absorption coefficient at the near edge absorption and that always average value in published table. Our results showed a wide range of data, the total measured data of mass-absorption coefficient of the seven elements was about 505. The investigation confirmed that XANES is useful technique for multi-element absorption coefficient measurement. Details of experimental methods and results are given and discussed. The experimental work has been performed at Beijing Synchrotron Radiation Facility. The measured values were compared with the published data. Good agreement between experimental results and published data is obtained.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Cheng-Jun, E-mail: cjsun@aps.anl.gov; Brewe, Dale L.; Heald, Steve M.

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorptionmore » near edge structure for Pr{sub 0.67}Sr{sub 0.33}MnO{sub 3} film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.« less

CSI 2264: Simultaneous optical and X-ray variability in pre-main sequence stars. I. Time resolved X-ray spectral analysis during optical dips and accretion bursts in stars with disks

NASA Astrophysics Data System (ADS)

Guarcello, M. G.; Flaccomio, E.; Micela, G.; Argiroffi, C.; Sciortino, S.; Venuti, L.; Stauffer, J.; Rebull, L.; Cody, A. M.

2017-06-01

Context. Pre-main sequence stars are variable sources. The main mechanisms responsible for their variability are variable extinction, unsteady accretion, and rotational modulation of both hot and dark photospheric spots and X-ray-active regions. In stars with disks, this variability is related to the morphology of the inner circumstellar region (≤0.1 AU) and that of the photosphere and corona, all impossible to be spatially resolved with present-day techniques. This has been the main motivation for the Coordinated Synoptic Investigation of NGC 2264, a set of simultaneous observations of NGC 2264 with 15 different telescopes. Aims: In this paper, we focus on the stars with disks. We analyze the X-ray spectral properties extracted during optical bursts and dips in order to unveil the nature of these phenomena. Stars without disks are studied in a companion paper. Methods: We analyze simultaneous CoRoT and Chandra/ACIS-I observations to search for coherent optical and X-ray flux variability in stars with disks. Then, stars are analyzed in two different samples. In stars with variable extinction, we look for a simultaneous increase of optical extinction and X-ray absorption during the optical dips; in stars with accretion bursts, we search for soft X-ray emission and increasing X-ray absorption during the bursts. Results: We find evidence for coherent optical and X-ray flux variability among the stars with variable extinction. In 9 of the 24 stars with optical dips, we observe a simultaneous increase of X-ray absorption and optical extinction. In seven dips, it is possible to calculate the NH/AV ratio in order to infer the composition of the obscuring material. In 5 of the 20 stars with optical accretion bursts, we observe increasing soft X-ray emission during the bursts that we associate to the emission of accreting gas. It is not surprising that these properties are not observed in all the stars with dips and bursts, since favorable geometric configurations are required. Conclusions: The observed variable absorption during the dips is mainly due to dust-free material in accretion streams. In stars with accretion bursts, we observe, on average, a larger soft X-ray spectral component not observed in non-accreting stars.

Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

DOE PAGES

Miaja-Avila, L.; O'Neil, G. C.; Uhlig, J.; ...

2015-03-02

We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ~10 6 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >10 7 laser pulses, wemore » also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.« less

X-ray scattering and spectroscopy studies on diesel soot from oxygenated fuel under various engine load conditions

USGS Publications Warehouse

Braun, Andreas; Shah, N.; Huggins, Frank E.; Kelly, K.E.; Sarofim, A.; Jacobsen, C.; Wirick, S.; Francis, H.; Ilavsky, J.; Thomas, G.E.; Huffman, G.P.

2005-01-01

Diesel soot from reference diesel fuel and oxygenated fuel under idle and load engine conditions was investigated with X-ray scattering and X-ray carbon K-edge absorption spectroscopy. Up to five characteristic size ranges were found. Idle soot was generally found to have larger primary particles and aggregates but smaller crystallites, than load soot. Load soot has a higher degree of crystallinity than idle soot. Adding oxygenates to diesel fuel enhanced differences in the characteristics of diesel soot, or even reversed them. Aromaticity of idle soot from oxygenated diesel fuel was significantly larger than from the corresponding load soot. Carbon near-edge X-ray absorption fine structure (NEXAFS) spectroscopy was applied to gather information about the presence of relative amounts of carbon double bonds (CC, CO) and carbon single bonds (C-H, C-OH, COOH). Using scanning X-ray transmission microspectroscopy (STXM), the relative amounts of these carbon bond states were shown to vary spatially over distances approximately 50 to 100 nm. The results from the X-ray techniques are supported by thermo-gravimetry analysis and high-resolution transmission electron microscopy. ?? 2005 Elsevier Ltd. All rights reserved.

High-definition X-ray fluorescence elemental mapping of paintings.

PubMed

Howard, Daryl L; de Jonge, Martin D; Lau, Deborah; Hay, David; Varcoe-Cocks, Michael; Ryan, Chris G; Kirkham, Robin; Moorhead, Gareth; Paterson, David; Thurrowgood, David

2012-04-03

A historical self-portrait painted by Sir Arthur Streeton (1867-1943) has been studied with fast-scanning X-ray fluorescence microscopy using synchrotron radiation. One of the technique's unique strengths is the ability to reveal metal distributions in the pigments of underlying brushstrokes, thus providing information critical to the interpretation of a painting. We have applied the nondestructive technique with the event-mode Maia X-ray detector, which has the capability to record elemental maps at megapixels per hour with the full X-ray fluorescence spectrum collected per pixel. The painting poses a difficult challenge to conventional X-ray analysis, because it was completely obscured with heavy brushstrokes of highly X-ray absorptive lead white paint (2PbCO(3)·Pb(OH)(2)) by the artist, making it an excellent candidate for the application of the synchrotron-based technique. The 25 megapixel elemental maps were successfully observed through the lead white paint across the 200 × 300 mm(2) scan area. The sweeping brushstrokes of the lead white overpaint contributed significant detrimental structure to the elemental maps. A corrective procedure was devised to enhance the visualization of the elemental maps by using the elastic X-ray scatter as a proxy for the lead white overpaint. We foresee the technique applied to the most demanding of culturally significant artworks where conventional analytical methods are inadequate.

Einstein X-ray observations of QSO's with absorption-line systems

NASA Technical Reports Server (NTRS)

Junkkarinen, V. T.; Marscher, A. P.; Burbidge, E. M.

1982-01-01

The detection of X-ray emission from eight QSO's is reported, plus an upper limit to the X-ray flux from one QSO, using the Einstein X-ray Observatory (HEAO-2). Each object in the sample contains at least one absorption-line system that has been identified in its optical spectrum. The present results are combined with those of other investigators to form a sample of 44 absorption-line QSO's (with 2 sub e greater than 1.2) which have been observed in the X-ray. This sample cannot be distinguished, in terms of X-ray properties, from one which consists of QSO's in which no absorption systems have been identified. These results are consistent with extrinsic models for absorption-line clouds, as well as with current versions of intrinsic models.

Identification of Uranyl Minerals Using Oxygen K-Edge X Ray Absorption Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ward, Jesse D.; Bowden, Mark E.; Resch, Charles T.

2016-03-01

Uranium analysis is consistently needed throughout the fuel cycle, from mining to fuel fabrication to environmental monitoring. Although most of the world’s uranium is immobilized as pitchblende or uraninite, there exists a plethora of secondary uranium minerals, nearly all of which contain the uranyl cation. Analysis of uranyl compounds can provide clues as to a sample’s facility of origin and chemical history. X-ray absorption spectroscopy is one technique that could enhance our ability to identify uranium minerals. Although there is limited chemical information to be gained from the uranium X-ray absorption edges, recent studies have successfully used ligand NEXAFS tomore » study the physical chemistry of various uranium compounds. This study extends the use of ligand NEXAFS to analyze a suite of uranium minerals. We find that major classes of uranyl compounds (carbonate, oxyhydroxide, silicate, and phosphate) exhibit characteristic lineshapes in the oxygen K-edge absorption spectra. As a result, this work establishes a library of reference spectra that can be used to classify unknown uranyl minerals.« less

[Experimental study and correction of the absorption and enhancement effect between Ti, V and Fe].

PubMed

Tuo, Xian-Guo; Mu, Ke-Liang; Li, Zhe; Wang, Hong-Hui; Luo, Hui; Yang, Jian-Bo

2009-11-01

The absorption and enhancement effects in X-ray fluorescence analysis for Ti, V and Fe elements were studied in the present paper. Three bogus duality systems of Ti-V/Ti-Fe/V-Fe samples were confected and measured by X-ray fluorescence analysis technique using HPGe semiconductor detector, and the relation curve between unitary coefficient (R(K)) of element count rate and element content (W(K)) were obtained after the experiment. Having analyzed the degree of absorption and enhancement effect between every two elements, the authors get the result, and that is the absorption and enhancement effect between Ti and V is relatively distinctness, while it's not so distinctness in Ti-Fe and V-Fe. After that, a mathematics correction method of exponential fitting was used to fit the R(K)-W(K) curve and get a function equation of X-ray fluorescence count rate and content. Three groups of Ti-V duality samples were used to test the fitting method and the relative errors of Ti and V were less than 0.2% as compared to the actual results.

Gold nanoclusters as contrast agents for fluorescent and X-ray dual-modality imaging.

PubMed

Zhang, Aili; Tu, Yu; Qin, Songbing; Li, Yan; Zhou, Juying; Chen, Na; Lu, Qiang; Zhang, Bingbo

2012-04-15

Multimodal imaging technique is an alternative approach to improve sensitivity of early cancer diagnosis. In this study, highly fluorescent and strong X-ray absorption coefficient gold nanoclusters (Au NCs) are synthesized as dual-modality imaging contrast agents (CAs) for fluorescent and X-ray dual-modality imaging. The experimental results show that the as-prepared Au NCs are well constructed with ultrasmall sizes, reliable fluorescent emission, high computed tomography (CT) value and fine biocompatibility. In vivo imaging results indicate that the obtained Au NCs are capable of fluorescent and X-ray enhanced imaging. Copyright © 2012 Elsevier Inc. All rights reserved.

Effects of gamma-ray irradiation on the optical properties of amorphous Se100-xHgx thin films

NASA Astrophysics Data System (ADS)

Ahmad, Shabir; Islam, Shama; Nasir, Mohd.; Asokan, K.; Zulfequar, M.

2018-06-01

In this study, the thermal quenching technique was employed to prepare bulk samples of Se100-xHgx (x = 0, 5, 10, 15). Thin films with a thickness of ∼250 nm were deposited on glass substrates using the thermal evaporation technique. These films were irradiated with gamma rays at doses of 25-100 kGy. The elemental compositions of the as-deposited thin films were confirmed by energy dispersive X-ray analysis and Rutherford backscattering spectrometry. X-ray diffraction analysis confirmed the crystalline nature of these thin films upto the dose of 75 kGy. Fourier transform-infrared spectroscopy showed that the concentration of defects decreased after gamma irradiation. Microstructural analysis by field emission scanning electron microscopy indicated that the grain size increases after irradiation. Optical study based on spectrophotometry showed that the optical band gap values of these films increase after the addition of Hg whereas they decrease after gamma irradiation. We found that the absorption coefficient increases with doses up to 75 kGy but decreases at higher doses. These remarkable shifts in the optical band gap and absorption coefficient values are interpreted in terms of the creation and annihilation of defects, which are the main effects produced by gamma irradiation.

Novel applications of X-ray photoelectron spectroscopy on unsupported nanoparticles

NASA Astrophysics Data System (ADS)

Kostko, Oleg; Xu, Bo; Jacobs, Michael I.; Ahmed, Musahid

X-ray photoelectron spectroscopy (XPS) is a powerful technique for chemical analysis of surfaces. We will present novel results of XPS on unsupported, gas-phase nanoparticles using a velocity-map imaging (VMI) spectrometer. This technique allows for probes of both the surfaces of nanoparticles via XPS as well as their interiors via near edge X-ray absorption fine structure (NEXAFS) spectroscopy. A recent application of this technique has confirmed that arginine's guanidinium group exists in a protonated state even in strongly basic solution. Moreover, the core-level photoelectron spectroscopy can provide information on the effective attenuation length (EAL) of low kinetic energy electrons. This contradictory value is important for determining the probing depth of XPS and in photolithography. A new method for determining EALs will be presented.

Forcing Cesium into Higher Oxidation States Using Useful hard x-ray Induced Chemistry under High Pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sneed, D.; Pravica, M.; Kim, E.

This paper discusses our attempt to synthesize higher oxidation forms of cesium fluoride by pressurizing cesium fluoride in a fluorine-rich environment created via the x-ray decomposition of potassium tetrafluoroborate. This was done in order to confirm recent theoretical predictions of higher oxidation forms of CsFn. We discuss the development of a technique to produce molecular fluorine in situ via useful hard x-ray photochemistry, and the attempt to utilize this technique to form higher oxidation states of cesium fluoride. In order to verify the formation of the novel stoichiometric species of CsFn. X-ray Absorption Near Edge Spectroscopy (XANES) centered on themore » cesium K-edge was performed to probe the oxidation state of cesium as well as the local molecular coordination around Cs.« less

In situ spectroscopy and spectroelectrochemistry of uranium in high-temperature alkali chloride molten salts.

PubMed

Polovov, Ilya B; Volkovich, Vladimir A; Charnock, John M; Kralj, Brett; Lewin, Robert G; Kinoshita, Hajime; May, Iain; Sharrad, Clint A

2008-09-01

Soluble uranium chloride species, in the oxidation states of III+, IV+, V+, and VI+, have been chemically generated in high-temperature alkali chloride melts. These reactions were monitored by in situ electronic absorption spectroscopy. In situ X-ray absorption spectroscopy of uranium(VI) in a molten LiCl-KCl eutectic was used to determine the immediate coordination environment about the uranium. The dominant species in the melt was [UO 2Cl 4] (2-). Further analysis of the extended X-ray absorption fine structure data and Raman spectroscopy of the melts quenched back to room temperature indicated the possibility of ordering beyond the first coordination sphere of [UO 2Cl 4] (2-). The electrolytic generation of uranium(III) in a molten LiCl-KCl eutectic was also investigated. Anodic dissolution of uranium metal was found to be more efficient at producing uranium(III) in high-temperature melts than the cathodic reduction of uranium(IV). These high-temperature electrolytic processes were studied by in situ electronic absorption spectroelectrochemistry, and we have also developed in situ X-ray absorption spectroelectrochemistry techniques to probe both the uranium oxidation state and the uranium coordination environment in these melts.

Structure of the manganese complex in photosystem II: insights from X-ray spectroscopy.

PubMed Central

Yachandra, Vittal K

2002-01-01

We have used Mn K-edge absorption and Kbeta emission spectroscopy to determine the oxidation states of the Mn complex in the various S states. We have started exploring the new technique of resonant inelastic X-ray scattering spectroscopy; this technique can be characterized as a Raman process that uses K-edge energies (1s to 4p, ca. 6550 eV) to obtain L-edge-like spectra (2p to 3d, ca. 650 eV). The relevance of these data to the oxidation states and structure of the Mn complex is presented. We have obtained extended X-ray absorption fine structure data from the S(0) and S(3) states and observed heterogeneity in the Mn-Mn distances leading us to conclude that there may be three rather than two di-mu-oxo-bridged units present per tetranuclear Mn cluster. In addition, we have obtained data using Ca and Sr X-ray spectroscopy that provide evidence for a heteronuclear Mn-Ca cluster. The possibility of three di-mu-oxo-bridged Mn-Mn moieties and the proximity of Ca is incorporated into developing structural models for the Mn cluster. The involvement of bridging and terminal O ligands of Mn in the mechanism of oxygen evolution is discussed in the context of our X-ray spectroscopy results. PMID:12437873

First-Principles Predictions of Near-Edge X-ray Absorption Fine Structure Spectra of Semiconducting Polymers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Su, Gregory M.; Patel, Shrayesh N.; Pemmaraju, C. D.

The electronic structure and molecular orientation of semiconducting polymers in thin films determine their ability to transport charge. Methods based on near-edge X-ray absorption fine structure (NEXAFS) spectroscopy can be used to probe both the electronic structure and microstructure of semiconducting polymers in both crystalline and amorphous films. However, it can be challenging to interpret NEXAFS spectra on the basis of experimental data alone, and accurate, predictive calculations are needed to complement experiments. Here, we show that first-principles density functional theory (DFT) can be used to model NEXAFS spectra of semiconducting polymers and to identify the nature of transitions inmore » complicated NEXAFS spectra. Core-level X-ray absorption spectra of a set of semiconducting polymers were calculated using the excited electron and core-hole (XCH) approach based on constrained-occupancy DFT. A comparison of calculations on model oligomers and periodic structures with experimental data revealed the requirements for accurate prediction of NEXAFS spectra of both conjugated homopolymers and donor–acceptor polymers. The NEXAFS spectra predicted by the XCH approach were applied to study molecular orientation in donor–acceptor polymers using experimental spectra and revealed the complexity of using carbon edge spectra in systems with large monomeric units. The XCH approach has sufficient accuracy in predicting experimental NEXAFS spectra of polymers that it should be considered for design and analysis of measurements using soft X-ray techniques, such as resonant soft X-ray scattering and scanning transmission X-ray microscopy.« less

The Advanced Light Source (ALS) Slicing Undulator Beamline

DOE Office of Scientific and Technical Information (OSTI.GOV)

Heimann, P. A.; Glover, T. E.; Plate, D.

2007-01-19

A beamline optimized for the bunch slicing technique has been construction at the Advanced Light Source (ALS). This beamline includes an in-vacuum undulator, soft and hard x-ray beamlines and a femtosecond laser system. The soft x-ray beamline may operate in spectrometer mode, where an entire absorption spectrum is accumulated at one time, or in monochromator mode. The femtosecond laser system has a high repetition rate of 20 kHz to improve the average slicing flux. The performance of the soft x-ray branch of the ALS slicing undulator beamline will be presented.

Observation of Reverse Saturable Absorption of an X-ray Laser

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cho, B. I.; Cho, M. S.; Kim, M.

A nonlinear absorber in which the excited state absorption is larger than the ground state can undergo a process called reverse saturable absorption. It is a well-known phenomenon in laser physics in the optical regime, but is more difficult to generate in the x-ray regime, where fast nonradiative core electron transitions typically dominate the population kinetics during light matter interactions. Here, we report the first observation of decreasing x-ray transmission in a solid target pumped by intense x-ray free electron laser pulses. The measurement has been made below the K-absorption edge of aluminum, and the x-ray intensity ranges are 10more » 16 –10 17 W=cm 2. It has been confirmed by collisional radiative population kinetic calculations, underscoring the fast spectral modulation of the x-ray pulses and charge states relevant to the absorption and transmission of x-ray photons. The processes shown through detailed simulations are consistent with reverse saturable absorption, which would be the first observation of this phenomena in the x-ray regime. These light matter interactions provide a unique opportunity to investigate optical transport properties in the extreme state of matters, as well as affording the potential to regulate ultrafast x-ray freeelectron laser pulses.« less

Observation of Reverse Saturable Absorption of an X-ray Laser

DOE PAGES

Cho, B. I.; Cho, M. S.; Kim, M.; ...

2017-08-16

A nonlinear absorber in which the excited state absorption is larger than the ground state can undergo a process called reverse saturable absorption. It is a well-known phenomenon in laser physics in the optical regime, but is more difficult to generate in the x-ray regime, where fast nonradiative core electron transitions typically dominate the population kinetics during light matter interactions. Here, we report the first observation of decreasing x-ray transmission in a solid target pumped by intense x-ray free electron laser pulses. The measurement has been made below the K-absorption edge of aluminum, and the x-ray intensity ranges are 10more » 16 –10 17 W=cm 2. It has been confirmed by collisional radiative population kinetic calculations, underscoring the fast spectral modulation of the x-ray pulses and charge states relevant to the absorption and transmission of x-ray photons. The processes shown through detailed simulations are consistent with reverse saturable absorption, which would be the first observation of this phenomena in the x-ray regime. These light matter interactions provide a unique opportunity to investigate optical transport properties in the extreme state of matters, as well as affording the potential to regulate ultrafast x-ray freeelectron laser pulses.« less

Time-resolved X-ray Absorption Spectroscopy for Electron Transport Study in Warm Dense Gold

NASA Astrophysics Data System (ADS)

Lee, Jong-Won; Bae, Leejin; Engelhorn, Kyle; Heimann, Philip; Ping, Yuan; Barbrel, Ben; Fernandez, Amalia; Beckwith, Martha Anne; Cho, Byoung-Ick; GIST Team; IBS Team; LBNL Collaboration; SLAC Collaboration; LLNL Collaboration

2015-11-01

The warm dense Matter represents states of which the temperature is comparable to Fermi energy and ions are strongly coupled. One of the experimental techniques to create such state in the laboratory condition is the isochoric heating of thin metal foil with femtosecond laser pulses. This concept largely relies on the ballistic transport of electrons near the Fermi-level, which were mainly studied for the metals in ambient conditions. However, they were barely investigated in warm dense conditions. We present a time-resolved x-ray absorption spectroscopy measured for the Au/Cu dual layered sample. The front Au layer was isochorically heated with a femtosecond laser pulse, and the x-ray absorption changes around L-edge of Cu, which was attached on the backside of Au, was measured with a picosecond resolution. Time delays between the heating of the `front surface' of Au layer and the alternation of x-ray spectrum of Cu attached on the `rear surface' of Au indicate the energetic electron transport mechanism through Au in the warm dense conditions. IBS (IBS-R012-D1) and the NRF (No. 2013R1A1A1007084) of Korea.

Identifying anthropogenic uranium compounds using soft X-ray near-edge absorption spectroscopy

NASA Astrophysics Data System (ADS)

Ward, Jesse D.; Bowden, Mark; Tom Resch, C.; Eiden, Gregory C.; Pemmaraju, C. D.; Prendergast, David; Duffin, Andrew M.

2017-01-01

Uranium ores mined for industrial use are typically acid-leached to produce yellowcake and then converted into uranium halides for enrichment and purification. These anthropogenic chemical forms of uranium are distinct from their mineral counterparts. The purpose of this study is to use soft X-ray absorption spectroscopy to characterize several common anthropogenic uranium compounds important to the nuclear fuel cycle. Chemical analyses of these compounds are important for process and environmental monitoring. X-ray absorption techniques have several advantages in this regard, including element-specificity, chemical sensitivity, and high spectral resolution. Oxygen K-edge spectra were collected for uranyl nitrate, uranyl fluoride, and uranyl chloride, and fluorine K-edge spectra were collected for uranyl fluoride and uranium tetrafluoride. Interpretation of the data is aided by comparisons to calculated spectra. The effect of hydration state on the sample, a potential complication in interpreting oxygen K-edge spectra, is discussed. These compounds have unique spectral signatures that can be used to identify unknown samples.

X-ray absorption near-edge spectroscopy in bioinorganic chemistry: Application to M–O2 systems

PubMed Central

Sarangi, Ritimukta

2012-01-01

Metal K-edge X-ray absorption spectroscopy (XAS) has been extensively applied to bioinorganic chemistry to obtain geometric structure information on metalloprotein and biomimetic model complex active sites by analyzing the higher energy extended X-ray absorption fine structure (EXAFS) region of the spectrum. In recent years, focus has been on developing methodologies to interpret the lower energy K-pre-edge and rising-edge regions (XANES) and using it for electronic structure determination in complex bioinorganic systems. In this review, the evolution and progress of 3d-transition metal K-pre-edge and rising-edge methodology development is presented with particular focus on applications to bioinorganic systems. Applications to biomimetic transition metal–O2 intermediates (M = Fe, Co, Ni and Cu) are reviewed, which demonstrate the power of the method as an electronic structure determination technique and its impact in understanding the role of supporting ligands in tuning the electronic configuration of transition metal–O2 systems. PMID:23525635

Soft X-ray characterization technique for Li batteries under operating conditions.

PubMed

Petersburg, Cole F; Daniel, Robert C; Jaye, Cherno; Fischer, Daniel A; Alamgir, Faisal M

2009-09-01

O K-edge and Co L-edge near-edge X-ray absorption fine structure has been used to examine the cathode of an intact solid-state lithium ion battery. The novel technique allowed for the simultaneous acquisition of partial electron yield and fluorescence yield data during the first charge cycle of a LiCoO(2)-based battery below the intercalation voltage. The chemical environments of oxygen and cobalt at the surface are shown to differ chemically from those in the bulk. The present design enables a wide variety of in situ spectroscopies, microscopies and scattering techniques.

Using acoustic levitation in synchrotron based laser pump hard x-ray probe experiments

NASA Astrophysics Data System (ADS)

Hu, Bin; Lerch, Jason; Suthar, Kamlesh; Dichiara, Anthony

Acoustic levitation provides a platform to trap and hold a small amount of material by using standing pressure waves without a container. The technique has a potential to be used for laser pump x-ray probe experiments; x-ray scattering and laser distortion from the container can be avoided, sample consumption can be minimized, and unwanted chemistry that may occur at the container interface can be avoided. The method has been used at synchrotron sources for studying protein and pharmaceutical solutions using x-ray diffraction (XRD) and small angle x-ray scattering (SAXS). However, pump-probe experiments require homogeneously excited samples, smaller than the absorption depth of the material that must be held stably at the intersection of both the laser and x-ray beams. We discuss 1) the role of oscillations in acoustic levitation and the optimal acoustic trapping conditions for x-ray/laser experiments, 2) opportunities to automate acoustic levitation for fast sample loading and manipulation, and 3) our experimental results using SAXS to monitor laser induced thermal expansion in gold nanoparticles solution. We also performed Finite Element Analysis to optimize the trapping performance and stability of droplets ranging from 0.4 mm to 2 mm. Our early x-ray/laser demonstrated the potential of the technique for time-resolved X-ray science.

Ultrafast X-Ray Absorption Spectroscopy of Isochorically Heated Warm Dense Matter

NASA Astrophysics Data System (ADS)

Engelhorn, Kyle Craig

This dissertation will present a series of new tools, together with new techniques, focused on the understanding of warm and dense matter. We report on the development of a high time resolution and high detection efficiency x-ray camera. The camera is integrated with a short pulse laser and an x-ray beamline at the Advanced Light Source synchrotron. This provides an instrument for single shot, broadband x-ray absorption spectroscopy of warm and dense matter with 2 picosecond time resolution. Warm and dense matter is created by isochorically heating samples of known density with an ultrafast optical laser pulse, and X-ray absorption spectroscopy probes the unoccupied electronic density of states before the onset of hydrodynamic expansion and electron-ion equilibrium is reached. Measured spectra from a variety of materials are compared with first principle molecular dynamics and density functional theory calculations. In heated silicon dioxide spectra, two novel pre-edge features are observed, a peak below the band gap and absorption within the band gap, while a reduction was observed in the features above the edge. From consideration of the calculated spectra, the peak below the gap is attributed to valence electrons that have been promoted to the conduction band, the absorption within the gap is attributed to broken Si-O bonds, and the reduction above the edge is attributed to an elevated ionic temperature. In heated copper spectra, a time-dependent shift and broadening of the absorption edge are observed, consistent with and elevated electron temperature. The temporal evolution of the electronic temperature is accurately determined by fitting the measured spectra with calculated spectra. The electron-ion equilibration is studied with a two-temperature model. In heated nickel spectra, a shift of the absorption edge is observed. This shift is found to be inconsistent with calculated spectra and independent of incident laser fluence. A shift of the chemical potential is applied to the calculated spectra to obtain satisfactory agreement with measured spectra.

X-ray diffraction microscopy on frozen hydrated specimens

NASA Astrophysics Data System (ADS)

Nelson, Johanna

X-rays are excellent for imaging thick samples at high resolution because of their large penetration depth compared to electrons and their short wavelength relative to visible light. To image biological material, the absorption contrast of soft X-rays, especially between the carbon and oxygen K-shell absorption edges, can be utilized to give high contrast, high resolution images without the need for stains or labels. Because of radiation damage and the desire for high resolution tomography, live cell imaging is not feasible. However, cells can be frozen in vitrified ice, which reduces the effect of radiation damage while maintaining their natural hydrated state. X-ray diffraction microscopy (XDM) is an imaging technique which eliminates the limitations imposed by current focusing optics simply by removing them entirely. Far-field coherent diffraction intensity patterns are collected on a pixelated detector allowing every scattered photon to be collected within the limits of the detector's efficiency and physical size. An iterative computer algorithm is then used to invert the diffraction intensity into a real space image with both absorption and phase information. This technique transfers the emphasis away from fabrication and alignment of optics, and towards data processing. We have used this method to image a pair of freeze-dried, immuno-labeled yeast cells to the highest resolution (13 nm) yet obtained for a whole eukaryotic cell. We discuss successes and challenges in working with frozen hydrated specimens and efforts aimed at high resolution imaging of vitrified eukaryotic cells in 3D.

TH-AB-209-07: High Resolution X-Ray-Induced Acoustic Computed Tomography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xiang, L; Tang, S; Ahmad, M

Purpose: X-ray radiographic absorption imaging is an invaluable tool in medical diagnostics, biology and materials science. However, the use of conventional CT is limited by two factors: the detection sensitivity to weak absorption material and the radiation dose from CT scanning. The purpose of this study is to explore X-ray induced acoustic computed tomography (XACT), a new imaging modality, which combines X-ray absorption contrast and high ultrasonic resolution to address these challenges. Methods: First, theoretical models was built to analyze the XACT sensitivity to X-ray absorption and calculate the minimal radiation dose in XACT imaging. Then, an XACT system comprisedmore » of an ultrashort X-ray pulse, a low noise ultrasound detector and a signal acquisition system was built to evaluate the X-ray induced acoustic signal generation. A piece of chicken bone and a phantom with two golden fiducial markers were exposed to 270 kVp X-ray source with 60 ns exposure time, and the X-ray induced acoustic signal was received by a 2.25MHz ultrasound transducer in 200 positions. XACT images were reconstructed by a filtered back-projection algorithm. Results: The theoretical analysis shows that X-ray induced acoustic signals have 100% relative sensitivity to X-ray absorption, but not to X-ray scattering. Applying this innovative technology to breast imaging, we can reduce radiation dose by a factor of 50 compared with newly FDA approved breast CT. The reconstructed images of chicken bone and golden fiducial marker phantom reveal that the spatial resolution of the built XACT system is 350µm. Conclusion: In XACT, the imaging sensitivity to X-ray absorption is improved and the imaging dose is dramatically reduced by using ultrashort pulsed X-ray. Taking advantage of the high ultrasonic resolution, we can also perform 3D imaging with a single X-ray pulse. This new modality has the potential to revolutionize x-ray imaging applications in medicine and biology.« less

Composition analysis of a polymer electrolyte membrane fuel cell microporous layer using scanning transmission X-ray microscopy and near edge X-ray absorption fine structure analysis

NASA Astrophysics Data System (ADS)

George, Michael G.; Wang, Jian; Banerjee, Rupak; Bazylak, Aimy

2016-03-01

The novel application of scanning transmission X-ray microscopy (STXM) to the microporous layer (MPL) of a polymer electrolyte membrane fuel cell is investigated. A spatially resolved chemical component distribution map is obtained for the MPL of a commercially available SGL 25 BC sample. This is achieved with near edge X-ray absorption fine structure spectroscopic analysis. Prior to analysis the sample is embedded in non-reactive epoxy and ultra-microtomed to a thickness of 100 nm. Polytetrafluoroethylene (PTFE), carbon particle agglomerates, and supporting epoxy resin distributions are identified and reconstructed for a scanning area of 6 μm × 6 μm. It is observed that the spatial distribution of PTFE is strongly correlated to the carbon particle agglomerations. Additionally, agglomerate structures of PTFE are identified, possibly indicating the presence of a unique mesostructure in the MPL. STXM analysis is presented as a useful technique for the investigation of chemical species distributions in the MPL.

TXM-Wizard: a program for advanced data collection and evaluation in full-field transmission X-ray microscopy

PubMed Central

Liu, Yijin; Meirer, Florian; Williams, Phillip A.; Wang, Junyue; Andrews, Joy C.; Pianetta, Piero

2012-01-01

Transmission X-ray microscopy (TXM) has been well recognized as a powerful tool for non-destructive investigation of the three-dimensional inner structure of a sample with spatial resolution down to a few tens of nanometers, especially when combined with synchrotron radiation sources. Recent developments of this technique have presented a need for new tools for both system control and data analysis. Here a software package developed in MATLAB for script command generation and analysis of TXM data is presented. The first toolkit, the script generator, allows automating complex experimental tasks which involve up to several thousand motor movements. The second package was designed to accomplish computationally intense tasks such as data processing of mosaic and mosaic tomography datasets; dual-energy contrast imaging, where data are recorded above and below a specific X-ray absorption edge; and TXM X-ray absorption near-edge structure imaging datasets. Furthermore, analytical and iterative tomography reconstruction algorithms were implemented. The compiled software package is freely available. PMID:22338691

Electron density and effective atomic number (Zeff) determination through x-ray Moiré deflectometry

NASA Astrophysics Data System (ADS)

Valdivia Leiva, Maria Pia; Stutman, Dan; Finkenthal, Michael

2014-10-01

Talbot-Lau based Moiré deflectometry is a powerful density diagnostic capable of delivering refraction information and attenuation from a single image, through the accurate detection of X-ray phase-shift and intensity. The technique is able to accurately measure both the real part of the index of refraction δ (directly related to electron density) and the attenuation coefficient μ of an object placed in the x-ray beam. Since the atomic number Z (or Zeff for a composite sample) is proportional to these quantities, an elemental map of the effective atomic number can be obtained with the ratio of the phase and the absorption image. The determination of Zeff from refraction and attenuation measurements with Moiré deflectometry could be of high interest in various fields of HED research such as shocked materials and ICF experiments as Zeff is linked, by definition, to the x-ray absorption properties of a specific material. This work is supported by U.S. DoE/NNSA Grant No. 435 DENA0001835.

High-order multilayer coated blazed gratings for high resolution soft x-ray spectroscopy

DOE PAGES

Voronov, Dmitriy L.; Goray, Leonid I.; Warwick, Tony; ...

2015-02-17

A grand challenge in soft x-ray spectroscopy is to drive the resolving power of monochromators and spectrometers from the 10 4 achieved routinely today to well above 10 5. This need is driven mainly by the requirements of a new technique that is set to have enormous impact in condensed matter physics, Resonant Inelastic X-ray Scattering (RIXS). Unlike x-ray absorption spectroscopy, RIXS is not limited by an energy resolution dictated by the core-hole lifetime in the excitation process. Using much higher resolving power than used for normal x-ray absorption spectroscopy enables access to the energy scale of soft excitations inmore » matter. These excitations such as magnons and phonons drive the collective phenomena seen in correlated electronic materials such as high temperature superconductors. RIXS opens a new path to study these excitations at a level of detail not formerly possible. However, as the process involves resonant excitation at an energy of around 1 keV, and the energy scale of the excitations one would like to see are at the meV level, to fully utilize the technique requires the development of monochromators and spectrometers with one to two orders of magnitude higher energy resolution than has been conventionally possible. Here we investigate the detailed diffraction characteristics of multilayer blazed gratings. These elements offer potentially revolutionary performance as the dispersive element in ultra-high resolution x-ray spectroscopy. In doing so, we have established a roadmap for the complete optimization of the grating design. Traditionally 1st order gratings are used in the soft x-ray region, but we show that as in the optical domain, one can work in very high spectral orders and thus dramatically improve resolution without significant loss in efficiency.« less

Use of synchrotron radiation to characterize metals in plants: the case of Cd in the hyperacumulator Arabidopsis halleri

NASA Astrophysics Data System (ADS)

Isaure, M.; Sarret, G.; Verbruggen, N.

2010-12-01

Phytoremediation uses plants to extract (phytoextraction) or stabilize (phytostabilization) metals accumulated in soils, and can be an alternative to invasive physico-chemical remediation techniques. Its development requires the knowledge of the mechanisms involved in metal tolerance and accumulation in plants, and particularly the way that plants transfer and store metals. In that context, synchrotron radiation based techniques such as micro-focused X-Ray Fluorescence (µXRF), and micro-focused X-ray Absorption Spectroscopy, including Extended X-ray Absorption Fine Structure and X-ray Absorption Near Edge Structure, are particularly suited to determine the localization and the chemical forms of metals in the different tissues, cells and sub-cellular compartments. Arabidopsis halleri is a Zn, Cd hyperaccumulating plant, naturally growing on contaminated sites, and is a model plant to investigate metal hyperaccumulation. This work presents the application of µXRF and Cd µXANES to determine the distribution and speciation of Cd in this species. Results showed that Cd was mainly located in the mesophyll and veins of leaves. It is bound to S ligands in some leaves and to O/N ligands in other ones, and the observed variations may be related to the age of the leaves. Cd speciation seems to differ from other metals, and particularly Zn, generally encountered in hyperaccumulators. High local Cd concentrations were also detected at the base of trichomes, epidermal hairs of leaves, associated to O/N ligands, probably to the cell wall. This phenomenon was also observed on non-hyperaccumulators and is clearly not the major sink for Cd, but trichomes might play a role in the detoxification process. This study illustrates the suitability of synchrotron radiation based techniques to investigate metal distribution and speciation in plants.

Conjugate observation of electron microburst groups by Bremsstrahlung X-ray and riometer techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Siren, J.C.; Rosenberg, T.J.; Detrick, D.

1980-12-01

The first evidence is reported of simultaneous conjugate electron microburst group precipitation. Groups of bremsstrahlung X ray microbursts (E>25 keV) were observed during a substorm recovery phase by a balloon-borne scintillation counter over Roberval, Quebec, Canada. The microburst groups were accompanied one-to-one by time-delayed and broadened pulses of ionospheric absorption measured by a high sensitivity 30-MHz riometer at Siple Station, Antarctica (Lapprox. =4.1). For the interval of highest correlation, the absolute lag between the two data sets was 4 +- 1 s, to the limit of the relative timing accuracy. Approximately 2 s of the observed lag had been introducesmore » by a low-pass filter in the riometer data acquistion unit. The remainder (2 s) was due to the ionospheric recombination process, which evidently had a response time (tauapprox.5 s) during this event much shorter than that ordinarily associated with the D region of the ionosphere. Model calculations of the ionspheric response to time-varying precipitation, derived from the profile of the measurement X ray flux, provide a consistent picture of simultaneous microburst group precipitation at conjugate points, absolute absorption and the electron spectrum derived from X rays, the degree of variation in absorption and X ray fluxes, and the characteristic ionospheric time constant at the altitude of maximum energy deposition.« less

X-ray absorption spectroscopy and X-ray photoelectron spectroscopy studies of CaSO 4:Dy thermoluminescent phosphors

NASA Astrophysics Data System (ADS)

Bakshi, A. K.; Jha, S. N.; Olivi, L.; Phase, D. M.; Kher, R. K.; Bhattacharyya, D.

2007-11-01

Extended X-ray absorption fine structure (EXAFS) measurements have been carried out on CaSO4:Dy phosphor samples at the Dy L3 edge with synchrotron radiation. Measurements were carried out on a set of samples which were subjected to post-preparation annealing at different temperatures and for different cycles. The EXAFS data have been analysed to find the Dy-S and Dy-O bond lengths in the neighbourhood of the Dy atoms in a CaSO4 matrix. The observations from EXAFS measurements were verified with XANES and XPS techniques. On the basis of these measurements, efforts were made to explain the loss of thermoluminescence sensitivity of CaSO4:Dy phosphors after repeated cycles of annealing at 400 °C in air for 1 h.

Effect of Zn2+, Fe3+ and Cr3+ addition to hydroxyapatite for its application as an active constituent of sunscreens

NASA Astrophysics Data System (ADS)

de Araujo, T. S.; de Souza, S. O.; de Sousa, E. M. B.

2010-11-01

Biocompatible phosphate materials are used in different applications like bone and dental implants, drug delivery systems and others, but could also be applied in inorganic sunscreens. Using sunscreens is extremely necessary, because long time exposure to sun can cause skin cancer. In this work chemical precipitation method has been used to produce hydroxyapatite. Cr3+, Zn2+ and Fe3+ doped samples were characterized using powder X-Ray Diffraction (XRD) and Optical Absorption techniques. X-ray diffraction measurements confirmed the materials were in the expected crystalline structures. The crystallite size as measured from the X-ray pattern was 23-27 nm (±1). The absorption spectra in the ultraviolet and visible ranges indicate that appropriately doped and sized hydroxyapatite particles may have potential applications as active constituents of sunscreens.

Delocalization and occupancy effects of 5f orbitals in plutonium intermetallics using L3-edge resonant X-ray emission spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Booth, C. H.; Medling, S. A.; Jiang, Yu

2014-06-24

Although actinide (An) L3 -edge X-ray absorption near-edge structure (XANES) spectroscopy has been very effective in determining An oxidation states in insulating, ionically bonded materials, such as in certain coordination compounds and mineral systems, the technique fails in systems featuring more delocalized 5f orbitals, especially in metals. Recently, actinide L3-edge resonant X-ray emission spec- troscopy (RXES) has been shown to be an effective alternative. This technique is further demonstrated here using a parameterized partial unoccupied density of states method to quantify both occupancy and delocalization of the 5f orbital in ?-Pu, ?-Pu, PuCoGa5 , PuCoIn5 , and PuSb2. These newmore » results, supported by FEFF calculations, highlight the effects of strong correlations on RXES spectra and the technique?s ability to differentiate between f-orbital occupation and delocalization.« less

Practical Problems in the Cement Industry Solved by Modern Research Techniques

ERIC Educational Resources Information Center

Daugherty, Kenneth E.; Robertson, Les D.

1972-01-01

Practical chemical problems in the cement industry are being solved by such techniques as infrared spectroscopy, gas chromatography-mass spectrometry, X-ray diffraction, atomic absorption and arc spectroscopy, thermally evolved gas analysis, Mossbauer spectroscopy, transmission and scanning electron microscopy. (CP)

High spatial resolution grain orientation and strain mapping in thin films using polychromatic submicron x-ray diffraction

NASA Astrophysics Data System (ADS)

Tamura, N.; MacDowell, A. A.; Celestre, R. S.; Padmore, H. A.; Valek, B.; Bravman, J. C.; Spolenak, R.; Brown, W. L.; Marieb, T.; Fujimoto, H.; Batterman, B. W.; Patel, J. R.

2002-05-01

The availability of high brilliance synchrotron sources, coupled with recent progress in achromatic focusing optics and large area two-dimensional detector technology, has allowed us to develop an x-ray synchrotron technique that is capable of mapping orientation and strain/stress in polycrystalline thin films with submicron spatial resolution. To demonstrate the capabilities of this instrument, we have employed it to study the microstructure of aluminum thin film structures at the granular and subgranular levels. Due to the relatively low absorption of x-rays in materials, this technique can be used to study passivated samples, an important advantage over most electron probes given the very different mechanical behavior of buried and unpassivated materials.

Reprint of: Combining theory and experiment for X-ray absorption spectroscopy and resonant X-ray scattering characterization of polymers

DOE PAGES

Su, Gregory M.; Cordova, Isvar A.; Brady, Michael A.; ...

2016-11-01

An improved understanding of fundamental chemistry, electronic structure, morphology, and dynamics in polymers and soft materials requires advanced characterization techniques that are amenable to in situ and operando studies. Soft X-ray methods are especially useful in their ability to non-destructively provide information on specific materials or chemical moieties. Analysis of these experiments, which can be very dependent on X-ray energy and polarization, can quickly become complex. Complementary modeling and predictive capabilities are required to properly probe these critical features. Here in this paper, we present relevant background on this emerging suite of techniques. We focus on how the combination ofmore » theory and experiment has been applied and can be further developed to drive our understanding of how these methods probe relevant chemistry, structure, and dynamics in soft materials.« less

Combining theory and experiment for X-ray absorption spectroscopy and resonant X-ray scattering characterization of polymers

DOE PAGES

Su, Gregory M.; Cordova, Isvar A.; Brady, Michael A.; ...

2016-07-04

We present that an improved understanding of fundamental chemistry, electronic structure, morphology, and dynamics in polymers and soft materials requires advanced characterization techniques that are amenable to in situ and operando studies. Soft X-ray methods are especially useful in their ability to non-destructively provide information on specific materials or chemical moieties. Analysis of these experiments, which can be very dependent on X-ray energy and polarization, can quickly become complex. Complementary modeling and predictive capabilities are required to properly probe these critical features. Here, we present relevant background on this emerging suite of techniques. Finally, we focus on how the combinationmore » of theory and experiment has been applied and can be further developed to drive our understanding of how these methods probe relevant chemistry, structure, and dynamics in soft materials.« less

Simulating Valence-to-Core X-ray Emission Spectroscopy of Transition Metal Complexes with Time-Dependent Density Functional Theory.

PubMed

Zhang, Yu; Mukamel, Shaul; Khalil, Munira; Govind, Niranjan

2015-12-08

Valence-to-core (VtC) X-ray emission spectroscopy (XES) has emerged as a powerful technique for the structural characterization of complex organometallic compounds in realistic environments. Since the spectrum represents electronic transitions from the ligand molecular orbitals to the core holes of the metal centers, the approach is more chemically sensitive to the metal-ligand bonding character compared with conventional X-ray absorption techniques. In this paper we study how linear-response time-dependent density functional theory (LR-TDDFT) can be harnessed to simulate K-edge VtC X-ray emission spectra reliably. LR-TDDFT allows one to go beyond the single-particle picture that has been extensively used to simulate VtC-XES. We consider seven low- and high-spin model complexes involving chromium, manganese, and iron transition metal centers. Our results are in good agreement with experiment.

Intensity-dependent resonant transmission of x-rays in solid-density aluminum plasma

NASA Astrophysics Data System (ADS)

Cho, M. S.; Chung, H.-K.; Cho, B. I.

2018-05-01

X-ray free-electron lasers (XFELs) provide unique opportunities to generate and investigate dense plasmas. The absorption and transmission properties of x-ray photons in dense plasmas are important in characterizing the state of the plasmas. Experimental evidence shows that the transmission of x-ray photons through dense plasmas depends greatly on the incident XFEL intensity. Here, we present a detailed analysis of intensity-dependent x-ray transmission in solid-density aluminum using collisional-radiative population kinetics calculations. Reverse saturable absorption (RSA), i.e., an increase in x-ray absorption with intensity has been observed for photon energies below the K-absorption edge and in the intensity range of 1016-1017 W/cm2 for XFEL photons with 1487 eV. At higher intensities, a transition from RSA to saturable absorption (SA) is predicted; thus, the x-ray absorption decreases with intensity above a threshold value. For XFEL photon energies of 1501 eV and 1515 eV, the transition from RSA to SA occurs at XFEL intensities between 1017-1018 W/cm2. Electron temperatures are predicted to be in the range of 30-50 eV for the given experimental conditions. Detailed population kinetics of the charge states explains the intensity-dependent absorption of x-ray photons and the fast modulation of XFEL pulses for both RSA and SA.

Phase contrast imaging of buccal mucosa tissues-Feasibility study

NASA Astrophysics Data System (ADS)

Fatima, A.; Tripathi, S.; Shripathi, T.; Kulkarni, V. K.; Banda, N. R.; Agrawal, A. K.; Sarkar, P. S.; Kashyap, Y.; Sinha, A.

2015-06-01

Phase Contrast Imaging (PCI) technique has been used to interpret physical parameters obtained from the image taken on the normal buccal mucosa tissue extracted from cheek of a patient. The advantages of this method over the conventional imaging techniques are discussed. PCI technique uses the X-ray phase shift at the edges differentiated by very minute density differences and the edge enhanced high contrast images reveal details of soft tissues. The contrast in the images produced is related to changes in the X-ray refractive index of the tissues resulting in higher clarity compared with conventional absorption based X-ray imaging. The results show that this type of imaging has better ability to visualize microstructures of biological soft tissues with good contrast, which can lead to the diagnosis of lesions at an early stage of the diseases.

AEGIS: Demographics of X-ray and Optically Selected Active Galactic Nuclei

NASA Astrophysics Data System (ADS)

Yan, Renbin; Ho, Luis C.; Newman, Jeffrey A.; Coil, Alison L.; Willmer, Christopher N. A.; Laird, Elise S.; Georgakakis, Antonis; Aird, James; Barmby, Pauline; Bundy, Kevin; Cooper, Michael C.; Davis, Marc; Faber, S. M.; Fang, Taotao; Griffith, Roger L.; Koekemoer, Anton M.; Koo, David C.; Nandra, Kirpal; Park, Shinae Q.; Sarajedini, Vicki L.; Weiner, Benjamin J.; Willner, S. P.

2011-02-01

We develop a new diagnostic method to classify galaxies into active galactic nucleus (AGN) hosts, star-forming galaxies, and absorption-dominated galaxies by combining the [O III]/Hβ ratio with rest-frame U - B color. This can be used to robustly select AGNs in galaxy samples at intermediate redshifts (z < 1). We compare the result of this optical AGN selection with X-ray selection using a sample of 3150 galaxies with 0.3 < z < 0.8 and I AB < 22, selected from the DEEP2 Galaxy Redshift Survey and the All-wavelength Extended Groth Strip International Survey. Among the 146 X-ray sources in this sample, 58% are classified optically as emission-line AGNs, the rest as star-forming galaxies or absorption-dominated galaxies. The latter are also known as "X-ray bright, optically normal galaxies" (XBONGs). Analysis of the relationship between optical emission lines and X-ray properties shows that the completeness of optical AGN selection suffers from dependence on the star formation rate and the quality of observed spectra. It also shows that XBONGs do not appear to be a physically distinct population from other X-ray detected, emission-line AGNs. On the other hand, X-ray AGN selection also has strong bias. About 2/3 of all emission-line AGNs at L bol > 1044 erg s-1 in our sample are not detected in our 200 ks Chandra images, most likely due to moderate or heavy absorption by gas near the AGN. The 2-7 keV detection rate of Seyfert 2s at z ~ 0.6 suggests that their column density distribution and Compton-thick fraction are similar to that of local Seyferts. Multiple sample selection techniques are needed to obtain as complete a sample as possible.

First-principles calculations of K-shell X-ray absorption spectra for warm dense nitrogen

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Zi; Zhang, Shen; Kang, Wei

2016-05-15

X-ray absorption spectrum is a powerful tool for atomic structure detection on warm dense matter. Here, we perform first-principles molecular dynamics and X-ray absorption spectrum calculations on warm dense nitrogen along a Hugoniot curve. From the molecular dynamics trajectory, the detailed atomic structures are examined for each thermodynamical condition. The K-shell X-ray absorption spectrum is calculated, and its changes with temperature and pressure along the Hugoniot curve are discussed. The warm dense nitrogen systems may contain isolated nitrogen atoms, N{sub 2} molecules, and nitrogen clusters, which show quite different contributions to the total X-ray spectrum due to their different electronmore » density of states. The changes of X-ray spectrum along the Hugoniot curve are caused by the different nitrogen structures induced by the temperature and the pressure. Some clear signatures on X-ray spectrum for different thermodynamical conditions are pointed out, which may provide useful data for future X-ray experiments.« less

Element Selectivity in Second-Harmonic Generation of GaFeO3 by a Soft-X-Ray Free-Electron Laser

NASA Astrophysics Data System (ADS)

Yamamoto, Sh.; Omi, T.; Akai, H.; Kubota, Y.; Takahashi, Y.; Suzuki, Y.; Hirata, Y.; Yamamoto, K.; Yukawa, R.; Horiba, K.; Yumoto, H.; Koyama, T.; Ohashi, H.; Owada, S.; Tono, K.; Yabashi, M.; Shigemasa, E.; Yamamoto, S.; Kotsugi, M.; Wadati, H.; Kumigashira, H.; Arima, T.; Shin, S.; Matsuda, I.

2018-06-01

Nonlinear optical frequency conversion has been challenged to move down to the extreme ultraviolet and x-ray region. However, the extremely low signals have allowed researchers to only perform transmission experiments of the gas phase or ultrathin films. Here, we report second harmonic generation (SHG) of the reflected beam of a soft x-ray free-electron laser from a solid, which is enhanced by the resonant effect. The observation revealed that the double resonance condition can be met by absorption edges for transition metal oxides in the soft x-ray range, and this suggests that the resonant SHG technique can be applicable to a wide range of materials. We discuss the possibility of element-selective SHG spectroscopy measurements in the soft x-ray range.

Study on Coloration Mechanism of Chinese Ancient Ceramics by X-ray Absorption Near-edge Structure

NASA Astrophysics Data System (ADS)

Peng, Y. H.; Xie, Z.; He, J. F.; Liu, Q. H.; Pan, Z. Y.; Cheng, W. R.; Wei, S. Q.

2013-04-01

The Fe K-edge X-ray absorption near-edge structure (XANES) spectra of a series of ceramic shards were measured by fluorescence mode to reveal the color-generating techniques of Chinese porcelain. The analysis disclosed relationships among the chemical form of the iron, the firing conditions and the colors of the ceramics. The results indicate that the coloration for different ceramics depend on the valence states of iron as the main color element in glaze and the proportion of Fe2+ and Fe3+ was attributed to the baking technology. The findings provide important information for archaeologist on the coloration researches.

Development of the surface-sensitive soft x-ray absorption fine structure measurement technique for the bulk insulator

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yonemura, Takumi, E-mail: yonemura-takumi@sei.co.jp; Iihara, Junji; Uemura, Shigeaki

We have succeeded in measuring X-ray absorption fine structure (TEY-XAFS) spectra of insulating plate samples by total electron yield. The biggest problem is how to suppress the charge-up. We have attempted to deposit a gold stripe electrode on the surface and obtained a TEY-XAFS spectrum. This indicates that the metal stripe electrode is very useful in the TEY-XAFS measurement of the insulating plate samples. In the detailed analysis, we have found that the effective area for suppressing charge-up was approximately 120 μm from the edge of the electrode.

Synchrotron-based XAS on structure investigation of La0.99-xSrx(Na, K, Ba)0.01MnO3 nanoparticles: Evidence of magnetic properties

NASA Astrophysics Data System (ADS)

Daengsakul, Sujittra; Saengplot, Saowalak; Kidkhunthod, Pinit; Pimsawat, Adulphan; Maensiri, Santi

2018-04-01

This work presents the structural study of La0.99-xSrx(Na, K, Ba)0.01MnO3 or LSAM nanoparticles synthesized using thermal-hydro decomposition method where A denotes Na, K, Sr and Ba, respectively. The effect of ionic radii size of A dopants or rA from the substitution of A for La and Sr on the MnO6 octrahedral structure, where the average size of the cations occupying in A-site or 〈rA〉 is fixed at ∼ 1.24 Å, is focused. The LSAM nanoparticles are carefully studied using X-ray diffraction (XRD) including Rietveld refinement and X-ray Absorption Spectroscopy (XAS) including X-ray Absorption Near edge Structure (XANES) and X-ray Absorption Fine Structure (EXAFS). The Rietveld refinement shows all nano-powder samples have rhombohedral structure. By XANES technique we found that the effect of A substitutions at A-site causes a slight change of mean oxidation state of Mn between 3.54 and 3.60. Furthermore, the structural distortion of MnO6 octrahedral in samples is analysed and obtained from EXAFS. The observed trend of ferromagnetism for all LSAM samples can be clearly explained by evidences of A-site doping, structural distortion around Mn atoms and mixing Mn3+/Mn4+ valence states.

Electronic structure and optical properties of CdSxSe1-x solid solution nanostructures from X-ray absorption near edge structure, X-ray excited optical luminescence, and density functional theory investigations

NASA Astrophysics Data System (ADS)

Murphy, M. W.; Yiu, Y. M.; Ward, M. J.; Liu, L.; Hu, Y.; Zapien, J. A.; Liu, Yingkai; Sham, T. K.

2014-11-01

The electronic structure and optical properties of a series of iso-electronic and iso-structural CdSxSe1-x solid solution nanostructures have been investigated using X-ray absorption near edge structure, extended X-ray absorption fine structure, and X-ray excited optical luminescence at various absorption edges of Cd, S, and Se. It is found that the system exhibits compositions, with variable local structure in-between that of CdS and CdSe accompanied by tunable optical band gap between that of CdS and CdSe. Theoretical calculation using density functional theory has been carried out to elucidate the observations. It is also found that luminescence induced by X-ray excitation shows new optical channels not observed previously with laser excitation. The implications of these observations are discussed.

Employing X-ray absorption technique for better detector resolution and measurement of low cross-section events

NASA Astrophysics Data System (ADS)

Sharma, Gaurav; Puri, Nitin K.; Kumar, Pravin; Nandi, T.

2018-03-01

The versatility of X-ray absorption technique is experimentally employed for enhancing the detector resolution and to rejuvenate the low probable transitions obscured in the pile-up region, during a beam-foil spectroscopy experiment. The multiple aluminum absorber layers (10 μm each) are used to suppress the pile-up contribution drastically and to restore a weak transition which is about 1.38 × 104 times weaker than a one-electron-one-photon transitions viz. Kα and Khα. The weak line is possibly originating from a two-electron-one-photon transition in He-like Ti. Further, the transitions, which were obscured in the spectra due to high intensity ratio, are revived by dissimilar line intensity attenuation using this technique. The measured lifetimes of Kα line with and without intensity attenuation match well within error bar. The present technique finds potential implications in understanding the structure of multiple-core-vacant ions and other low cross section processes in ion-solid collisions.

Ionized absorbers, ionized emitters, and the X-ray spectrum of active galactic nuclei

NASA Technical Reports Server (NTRS)

Netzer, Hagai

1993-01-01

Broad absorption features are common in the X-ray spectrum of low-luminosity AGNs. The features have been modeled by leaky neutral absorbers or by highly ionized gas that completely occult the continuum source. Such models are incomplete since they do not take into account all the physical processes in the gas. In particular, no previous model included the X-ray emission by the ionized absorbing gas and the reflection of the continuum source radiation. The present work discusses the emission, absorption, and reflection properties of photoionized gases with emphasis on conditions thought to prevail in AGNs. It shows that such gas is likely to produce intense X-ray line and continuum radiation and to reflect a sizable fraction of the nonstellar continuum at all energies. If such gas is indeed responsible for the observed X-ray absorption, then absorption edges are much weaker than commonly assumed, and some residual X-ray continuum is likely to be observed even if the line of sight is completely blocked. Moreover, X-ray emission features may show up in sources not showing X-ray absorption. This has immense consequences for medium-resolution X-ray missions, such as BBXRT and Astro-D, and for the planned high-resolution experiments on board XMM and AXAF.

Modern Progress and Modern Problems in High Resolution X-ray Absorption from the Cold Interstellar Medium

NASA Astrophysics Data System (ADS)

Corrales, Lia; Li, Haochuan; Heinz, Sebastian

2018-01-01

With accurate cross-sections and higher signal-to-noise, X-ray spectroscopy can directly measure Milky Way gas and dust-phase metal abundances with few underlying assumptions. The X-ray energy band is sensitive to absorption by all abundant interstellar metals — carbon, oxygen, neon, silicon, magnesium, and iron — whether they are in gas or dust form. High resolution X-ray spectra from Galactic X-ray point sources can be used to directly measure metal abundances from all phases of the interstellar medium (ISM) along singular sight lines. We show our progress for measuring the depth of photoelectric absorption edges from neutral ISM metals, using all the observations of bright Galactic X-ray binaries available in the Chandra HETG archive. The cross-sections we use take into account both the absorption and scattering effects by interstellar dust grains on the iron and silicate spectral features. However, there are many open problems for reconciling X-ray absorption spectroscopy with ISM observations in other wavelengths. We will review the state of the field, lab measurements needed, and ways in which the next generation of X-ray telescopes will contribute.

Chemical imaging analysis of the brain with X-ray methods

NASA Astrophysics Data System (ADS)

Collingwood, Joanna F.; Adams, Freddy

2017-04-01

Cells employ various metal and metalloid ions to augment the structure and the function of proteins and to assist with vital biological processes. In the brain they mediate biochemical processes, and disrupted metabolism of metals may be a contributing factor in neurodegenerative disorders. In this tutorial review we will discuss the particular role of X-ray methods for elemental imaging analysis of accumulated metal species and metal-containing compounds in biological materials, in the context of post-mortem brain tissue. X-rays have the advantage that they have a short wavelength and can penetrate through a thick biological sample. Many of the X-ray microscopy techniques that provide the greatest sensitivity and specificity for trace metal concentrations in biological materials are emerging at synchrotron X-ray facilities. Here, the extremely high flux available across a wide range of soft and hard X-rays, combined with state-of-the-art focusing techniques and ultra-sensitive detectors, makes it viable to undertake direct imaging of a number of elements in brain tissue. The different methods for synchrotron imaging of metals in brain tissues at regional, cellular, and sub-cellular spatial resolution are discussed. Methods covered include X-ray fluorescence for elemental imaging, X-ray absorption spectrometry for speciation imaging, X-ray diffraction for structural imaging, phase contrast for enhanced contrast imaging and scanning transmission X-ray microscopy for spectromicroscopy. Two- and three-dimensional (confocal and tomographic) imaging methods are considered as well as the correlation of X-ray microscopy with other imaging tools.

Characterization and speciation of mercury-bearing mine wastes using X-ray absorption spectroscopy

USGS Publications Warehouse

Kim, C.S.; Brown, Gordon E.; Rytuba, J.J.

2000-01-01

Mining of mercury deposits located in the California Coast Range has resulted in the release of mercury to the local environment and water supplies. The solubility, transport, and potential bioavailability of mercury are controlled by its chemical speciation, which can be directly determined for samples with total mercury concentrations greater than 100 mg kg-1 (ppm) using X-ray absorption spectroscopy (XAS). This technique has the additional benefits of being non-destructive to the sample, element-specific, relatively sensitive at low concentrations, and requiring minimal sample preparation. In this study, Hg L(III)-edge extended X-ray absorption fine structure (EXAFS) spectra were collected for several mercury mine tailings (calcines) in the California Coast Range. Total mercury concentrations of samples analyzed ranged from 230 to 1060 ppm. Speciation data (mercury phases present and relative abundances) were obtained by comparing the spectra from heterogeneous, roasted (calcined) mine tailings samples with a spectral database of mercury minerals and sorbed mercury complexes. Speciation analyses were also conducted on known mixtures of pure mercury minerals in order to assess the quantitative accuracy of the technique. While some calcine samples were found to consist exclusively of mercuric sulfide, others contain additional, more soluble mercury phases, indicating a greater potential for the release of mercury into solution. Also, a correlation was observed between samples from hot-spring mercury deposits, in which chloride levels are elevated, and the presence of mercury-chloride species as detected by the speciation analysis. The speciation results demonstrate the ability of XAS to identify multiple mercury phases in a heterogeneous sample, with a quantitative accuracy of ??25% for the mercury-containing phases considered. Use of this technique, in conjunction with standard microanalytical techniques such as X-ray diffraction and electron probe microanalysis, is beneficial in the prioritization and remediation of mercury-contaminated mine sites. (C) 2000 Elsevier Science B.V.

Evidence for Different Reaction Pathways for Liquid and Granular Micronutrients in a Calcareous Soil

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hettiarachchi, Ganga M.; McLaughlin, Mike J.; Scheckel, Kirk G.

2008-06-16

The benefits of Mn and Zn fluid fertilizers over conventional granular products in calcareous sandy loam soils have been agronomically demonstrated. We hypothesized that the differences in the effectiveness between granular and fluid Mn and Zn fertilizers is due to different Mn and Zn reaction processes in and around fertilizer granules and fluid fertilizer bands. We used a combination of several synchrotron-based x-ray techniques, namely, spatially resolved micro-x-ray fluorescence (?-XRF), micro-x-ray absorption near edge structure spectroscopy (?-XANES), and bulk-XANES and -extended x-ray absorption fine structure (EXAFS) spectroscopy, along with several laboratory-based x-ray techniques to speciate different fertilizer-derived Mn and Znmore » species in highly calcareous soils to understand the chemistry underlying the observed differential behavior of fluid and granular micronutrient forms. Micro-XRF mapping of soil-fertilizer reactions zones indicated that the mobility of Mn and Zn from liquid fertilizer was greater than that observed for equivalent granular sources of these micronutrients in soil. After application of these micronutrient fertilizers to soil, Mn and Zn from liquid fertilizers were found to remain in comparatively more soluble solid forms, such as hydrated Mn phosphate-like, Mn calcite-like, adsorbed Zn-like, and Zn silicate-like phases, whereas Mn and Zn from equivalent granular sources tended to transform into comparatively less soluble solid forms such as Mn oxide-like, Mn carbonate-like, and Zn phosphate-like phases.« less

Diffraction enhance x-ray imaging for quantitative phase contrast studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Agrawal, A. K.; Singh, B., E-mail: balwants@rrcat.gov.in; Kashyap, Y. S.

2016-05-23

Conventional X-ray imaging based on absorption contrast permits limited visibility of feature having small density and thickness variations. For imaging of weakly absorbing material or materials possessing similar densities, a novel phase contrast imaging techniques called diffraction enhanced imaging has been designed and developed at imaging beamline Indus-2 RRCAT Indore. The technique provides improved visibility of the interfaces and show high contrast in the image forsmall density or thickness gradients in the bulk. This paper presents basic principle, instrumentation and analysis methods for this technique. Initial results of quantitative phase retrieval carried out on various samples have also been presented.

An XMM Investigation of Non-Thermal Phenomena in the Winds of Early-Type Stars

NASA Technical Reports Server (NTRS)

Waldron, Wayne L.; Mushotzky, Richard (Technical Monitor)

2002-01-01

The X-ray emission from early-type stars is believed to arise from a stellar wind distribution of shocks. Hence, X-ray analyses of these stars must include the effects of stellar wind X-ray absorption, which, in general dominates the ISM absorption. Although the absorption cross sections for the wind and ISM are essentially identical above 1 keV, there is substantial differences below 1 keV. Typically, if one only uses ISM cross sections to obtain fits to X-ray spectra, the fits usually indicate a model deficiency at energies below 1 keV which is attributed to the large increase in ISM cross sections at these energies. This deficiency can be eliminated by using stellar wind absorption models with a fixed ISM component. Since all early-type stars have substantial X-ray emission below 1 keV, than inclusion of wind absorption has proven to be a critical component in fitting X-ray spectra at low energies, verifying that these X-rays are indeed arising from within the stellar wind.

Non-resonant inelastic x-ray scattering spectra of lithiated titanium oxides for battery applications

NASA Astrophysics Data System (ADS)

Nagle, Kenneth; Balasubramanian, Mali; Johnson, Christopher; Seidler, Gerald; Belharouak, Ilias

2008-03-01

Although lithium-ion batteries now see widespread use, there remain considerable questions concerning the basic solid state chemistry of both electrodes. Improved understanding of the local electronic structure, particularly the mechanism of charge transfer upon insertion and removal of lithium, could lead to innovation in battery design and improved performance. We present non-resonant inelastic x-ray scattering (NRIXS) spectra from 2p initial states in titanium; these spectra are among the first recorded for such states in a transition metal. These spectra were obtained using the lower energy resolution inelastic x-ray scattering (LERIX) spectrometer, which is capable of making simultaneous measurements at nineteen values of momentum transfer. We demonstrate the ability to obtain soft x-ray absorption-like information using a bulk-sensitive, hard x-ray technique. In addition, at high momentum transfer NRIXS provides information about non-dipole transitions that are inaccessible by soft x-ray spectroscopic methods.

CARNAÚBA: The Coherent X-Ray Nanoprobe Beamline for the Brazilian Synchrotron SIRIUS/LNLS

NASA Astrophysics Data System (ADS)

Tolentino, Hélio C. N.; Soares, Márcio M.; Perez, Carlos A.; Vicentin, Flávio C.; Abdala, Dalton B.; Galante, Douglas; Teixeira, Verônica de C.; de Araújo, Douglas H. C.; Westfahl, Harry, Jr.

2017-06-01

The CARNAÚBA beamline is the tender-to-hard X-ray (2 - 15 keV) scanning nanoprobe planned for the 4th generation storage ring SIRIUS at the LNLS. CARNAÚBA uses an undulator source with vertical linear polarization in a low-beta straight section and grazing incidence-focusing mirrors to create a nanoprobe at 143 m from the source. The beamline optic is based on KB mirrors and provides high brilliance at an achromatic focal spot down to the diffraction limit diameter of ˜30 nm with a working distance of ˜6 cm. These characteristics are crucial for studying nanometric samples in experiments involving complex stages and environments. The CARNAÚBA beamline aims to perform raster scans using x-ray fluorescence, x-ray absorption spectroscopy, x-ray diffraction and coherent x-ray imaging techniques. Computed tomography will extend these methods to three dimensions.

Understanding of sub-band gap absorption of femtosecond-laser sulfur hyperdoped silicon using synchrotron-based techniques

PubMed Central

Limaye, Mukta V.; Chen, S. C.; Lee, C. Y.; Chen, L. Y.; Singh, Shashi B.; Shao, Y. C.; Wang, Y. F.; Hsieh, S. H.; Hsueh, H. C.; Chiou, J. W.; Chen, C. H.; Jang, L. Y.; Cheng, C. L.; Pong, W. F.; Hu, Y. F.

2015-01-01

The correlation between sub-band gap absorption and the chemical states and electronic and atomic structures of S-hyperdoped Si have been extensively studied, using synchrotron-based x-ray photoelectron spectroscopy (XPS), x-ray absorption near-edge spectroscopy (XANES), extended x-ray absorption fine structure (EXAFS), valence-band photoemission spectroscopy (VB-PES) and first-principles calculation. S 2p XPS spectra reveal that the S-hyperdoped Si with the greatest (~87%) sub-band gap absorption contains the highest concentration of S2− (monosulfide) species. Annealing S-hyperdoped Si reduces the sub-band gap absorptance and the concentration of S2− species, but significantly increases the concentration of larger S clusters [polysulfides (Sn2−, n > 2)]. The Si K-edge XANES spectra show that S hyperdoping in Si increases (decreased) the occupied (unoccupied) electronic density of states at/above the conduction-band-minimum. VB-PES spectra evidently reveal that the S-dopants not only form an impurity band deep within the band gap, giving rise to the sub-band gap absorption, but also cause the insulator-to-metal transition in S-hyperdoped Si samples. Based on the experimental results and the calculations by density functional theory, the chemical state of the S species and the formation of the S-dopant states in the band gap of Si are critical in determining the sub-band gap absorptance of hyperdoped Si samples. PMID:26098075

An algebraic iterative reconstruction technique for differential X-ray phase-contrast computed tomography.

PubMed

Fu, Jian; Schleede, Simone; Tan, Renbo; Chen, Liyuan; Bech, Martin; Achterhold, Klaus; Gifford, Martin; Loewen, Rod; Ruth, Ronald; Pfeiffer, Franz

2013-09-01

Iterative reconstruction has a wide spectrum of proven advantages in the field of conventional X-ray absorption-based computed tomography (CT). In this paper, we report on an algebraic iterative reconstruction technique for grating-based differential phase-contrast CT (DPC-CT). Due to the differential nature of DPC-CT projections, a differential operator and a smoothing operator are added to the iterative reconstruction, compared to the one commonly used for absorption-based CT data. This work comprises a numerical study of the algorithm and its experimental verification using a dataset measured at a two-grating interferometer setup. Since the algorithm is easy to implement and allows for the extension to various regularization possibilities, we expect a significant impact of the method for improving future medical and industrial DPC-CT applications. Copyright © 2012. Published by Elsevier GmbH.

Are There Intrinsically X-Ray Quiet Quasars

NASA Technical Reports Server (NTRS)

Gallagher, S. C.; Brandt, W. N.; Laor, A.; Elvis, Martin; Mathur, S.; Wills, Beverly J.; Iyomoto, N.; White, Nicholas (Technical Monitor)

2000-01-01

Recent ROSAT studies have identified a significant population of Active Galactic Nuclei (AGN) that are notably faint in soft X-rays relative to their optical fluxes. Are these AGN intrinsically X-ray weak or are they just highly absorbed? Brandt, Laor & Wills have systematically examined the optical and UV spectral properties of a well-defined sample of these soft X-ray weak (SXW) AGN drawn from the Boroson & Green sample of all the Palomar Green AGN 00 with z < 0.5. We present ASCA observations of three of these SXW AGN: PG 1011-040, PG 1535+547 (Mrk 486), and PG 2112+059. In general, our ASCA observations support the intrinsic absorption scenario for explaining soft X-ray weakness; both PG 1535+547 and PG 2112+059 show significant column densities (NH is approximately 10(exp 22) - 10(exp 23)/sq cm) of absorbing gas. Interestingly, PG 1011-040 shows no spectral evidence for X-ray absorption. The weak X-ray emission may result from very strong absorption of a partially covered source, or this AGN may be intrinsically X-ray weak. PG 2112+059 is a Broad Absorption Line (BAL) QSO, and we find it to have the highest X-ray flux known of this class. It shows a typical power-law X-ray continuum above 3 keV; this is the first direct evidence that BAL QSOs indeed have normal X-ray continua underlying their intrinsic absorption. Finally, marked variability between the ROSAT and ASCA observations of PG 1535+547 and PG 2112+059 suggests that the soft X-ray weak designation may be transient, and multi-epoch 0.1-10.0 KeV X-ray observations are required to constrain variability of the absorber and continuum.

High quality x-ray absorption spectroscopy measurements with long energy range at high pressure using diamond anvil cell.

PubMed

Hong, Xinguo; Newville, Matthew; Prakapenka, Vitali B; Rivers, Mark L; Sutton, Stephen R

2009-07-01

We describe an approach for acquiring high quality x-ray absorption fine structure (XAFS) spectroscopy spectra with wide energy range at high pressure using diamond anvil cell (DAC). Overcoming the serious interference of diamond Bragg peaks is essential for combining XAFS and DAC techniques in high pressure research, yet an effective method to obtain accurate XAFS spectrum free from DAC induced glitches has been lacking. It was found that these glitches, whose energy positions are very sensitive to the relative orientation between DAC and incident x-ray beam, can be effectively eliminated using an iterative algorithm based on repeated measurements over a small angular range of DAC orientation, e.g., within +/-3 degrees relative to the x-ray beam direction. Demonstration XAFS spectra are reported for rutile-type GeO2 recorded by traditional ambient pressure and high pressure DAC methods, showing similar quality at 440 eV above the absorption edge. Accurate XAFS spectra of GeO2 glass were obtained at high pressure up to 53 GPa, providing important insight into the structural polymorphism of GeO2 glass at high pressure. This method is expected be applicable for in situ XAFS measurements using a diamond anvil cell up to ultrahigh pressures.

High quality x-ray absorption spectroscopy measurements with long energy range at high pressure using diamond anvil cell

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hong, X.; Newville, M.; Prakapenka, V.B.

We describe an approach for acquiring high quality x-ray absorption fine structure (XAFS) spectroscopy spectra with wide energy range at high pressure using diamond anvil cell (DAC). Overcoming the serious interference of diamond Bragg peaks is essential for combining XAFS and DAC techniques in high pressure research, yet an effective method to obtain accurate XAFS spectrum free from DAC induced glitches has been lacking. It was found that these glitches, whose energy positions are very sensitive to the relative orientation between DAC and incident x-ray beam, can be effectively eliminated using an iterative algorithm based on repeated measurements over amore » small angular range of DAC orientation, e.g., within {+-}3{sup o} relative to the x-ray beam direction. Demonstration XAFS spectra are reported for rutile-type GeO{sub 2} recorded by traditional ambient pressure and high pressure DAC methods, showing similar quality at 440 eV above the absorption edge. Accurate XAFS spectra of GeO{sub 2} glass were obtained at high pressure up to 53 GPa, providing important insight into the structural polymorphism of GeO{sub 2} glass at high pressure. This method is expected be applicable for in situ XAFS measurements using a diamond anvil cell up to ultrahigh pressures.« less

Elementary review of electron microprobe techniques and correction requirements

NASA Technical Reports Server (NTRS)

Hart, R. K.

1968-01-01

Report contains requirements for correction of instrumented data on the chemical composition of a specimen, obtained by electron microprobe analysis. A condensed review of electron microprobe techniques is presented, including background material for obtaining X ray intensity data corrections and absorption, atomic number, and fluorescence corrections.

A simple method of obtaining concentration depth-profiles from X-ray diffraction

NASA Technical Reports Server (NTRS)

Wiedemann, K. E.; Unnam, J.

1984-01-01

The construction of composition profiles from X-ray intensity bands was investigated. The intensity band-to-composition profile transformation utilizes a solution which can be easily evaluated. The technique can be applied to thin films and thick speciments for which the variation of lattice parameters, linear absorption coefficient, and reflectivity with composition are known. A deconvolution scheme with corrections for the instrumental broadening and ak-alfadoublet is discussed.

Terahertz in-line digital holography of human hepatocellular carcinoma tissue.

PubMed

Rong, Lu; Latychevskaia, Tatiana; Chen, Chunhai; Wang, Dayong; Yu, Zhengping; Zhou, Xun; Li, Zeyu; Huang, Haochong; Wang, Yunxin; Zhou, Zhou

2015-02-13

Terahertz waves provide a better contrast in imaging soft biomedical tissues than X-rays, and unlike X-rays, they cause no ionisation damage, making them a good option for biomedical imaging. Terahertz absorption imaging has conventionally been used for cancer diagnosis. However, the absorption properties of a cancerous sample are influenced by two opposing factors: an increase in absorption due to a higher degree of hydration and a decrease in absorption due to structural changes. It is therefore difficult to diagnose cancer from an absorption image. Phase imaging can thus be critical for diagnostics. We demonstrate imaging of the absorption and phase-shift distributions of 3.2 mm × 2.3 mm × 30-μm-thick human hepatocellular carcinoma tissue by continuous-wave terahertz digital in-line holography. The acquisition time of a few seconds for a single in-line hologram is much shorter than that of other terahertz diagnostic techniques, and future detectors will allow acquisition of meaningful holograms without sample dehydration. The resolution of the reconstructions was enhanced by sub-pixel shifting and extrapolation. Another advantage of this technique is its relaxed minimal sample size limitation. The fibrosis indicated in the phase distribution demonstrates the potential of terahertz holographic imaging to obtain a more objective, early diagnosis of cancer.

Terahertz in-line digital holography of human hepatocellular carcinoma tissue

PubMed Central

Rong, Lu; Latychevskaia, Tatiana; Chen, Chunhai; Wang, Dayong; Yu, Zhengping; Zhou, Xun; Li, Zeyu; Huang, Haochong; Wang, Yunxin; Zhou, Zhou

2015-01-01

Terahertz waves provide a better contrast in imaging soft biomedical tissues than X-rays, and unlike X-rays, they cause no ionisation damage, making them a good option for biomedical imaging. Terahertz absorption imaging has conventionally been used for cancer diagnosis. However, the absorption properties of a cancerous sample are influenced by two opposing factors: an increase in absorption due to a higher degree of hydration and a decrease in absorption due to structural changes. It is therefore difficult to diagnose cancer from an absorption image. Phase imaging can thus be critical for diagnostics. We demonstrate imaging of the absorption and phase-shift distributions of 3.2 mm × 2.3 mm × 30-μm-thick human hepatocellular carcinoma tissue by continuous-wave terahertz digital in-line holography. The acquisition time of a few seconds for a single in-line hologram is much shorter than that of other terahertz diagnostic techniques, and future detectors will allow acquisition of meaningful holograms without sample dehydration. The resolution of the reconstructions was enhanced by sub-pixel shifting and extrapolation. Another advantage of this technique is its relaxed minimal sample size limitation. The fibrosis indicated in the phase distribution demonstrates the potential of terahertz holographic imaging to obtain a more objective, early diagnosis of cancer. PMID:25676705

Terahertz in-line digital holography of human hepatocellular carcinoma tissue

NASA Astrophysics Data System (ADS)

Rong, Lu; Latychevskaia, Tatiana; Chen, Chunhai; Wang, Dayong; Yu, Zhengping; Zhou, Xun; Li, Zeyu; Huang, Haochong; Wang, Yunxin; Zhou, Zhou

2015-02-01

Terahertz waves provide a better contrast in imaging soft biomedical tissues than X-rays, and unlike X-rays, they cause no ionisation damage, making them a good option for biomedical imaging. Terahertz absorption imaging has conventionally been used for cancer diagnosis. However, the absorption properties of a cancerous sample are influenced by two opposing factors: an increase in absorption due to a higher degree of hydration and a decrease in absorption due to structural changes. It is therefore difficult to diagnose cancer from an absorption image. Phase imaging can thus be critical for diagnostics. We demonstrate imaging of the absorption and phase-shift distributions of 3.2 mm × 2.3 mm × 30-μm-thick human hepatocellular carcinoma tissue by continuous-wave terahertz digital in-line holography. The acquisition time of a few seconds for a single in-line hologram is much shorter than that of other terahertz diagnostic techniques, and future detectors will allow acquisition of meaningful holograms without sample dehydration. The resolution of the reconstructions was enhanced by sub-pixel shifting and extrapolation. Another advantage of this technique is its relaxed minimal sample size limitation. The fibrosis indicated in the phase distribution demonstrates the potential of terahertz holographic imaging to obtain a more objective, early diagnosis of cancer.

Refraction-enhanced backlit imaging of axially symmetric inertial confinement fusion plasmas.

PubMed

Koch, Jeffrey A; Landen, Otto L; Suter, Laurence J; Masse, Laurent P; Clark, Daniel S; Ross, James S; Mackinnon, Andrew J; Meezan, Nathan B; Thomas, Cliff A; Ping, Yuan

2013-05-20

X-ray backlit radiographs of dense plasma shells can be significantly altered by refraction of x rays that would otherwise travel straight-ray paths, and this effect can be a powerful tool for diagnosing the spatial structure of the plasma being radiographed. We explore the conditions under which refraction effects may be observed, and we use analytical and numerical approaches to quantify these effects for one-dimensional radial opacity and density profiles characteristic of inertial-confinement fusion (ICF) implosions. We also show how analytical and numerical approaches allow approximate radial plasma opacity and density profiles to be inferred from point-projection refraction-enhanced radiography data. This imaging technique can provide unique data on electron density profiles in ICF plasmas that cannot be obtained using other techniques, and the uniform illumination provided by point-like x-ray backlighters eliminates a significant source of uncertainty in inferences of plasma opacity profiles from area-backlit pinhole imaging data when the backlight spatial profile cannot be independently characterized. The technique is particularly suited to in-flight radiography of imploding low-opacity shells surrounding hydrogen ice, because refraction is sensitive to the electron density of the hydrogen plasma even when it is invisible to absorption radiography. It may also provide an alternative approach to timing shockwaves created by the implosion drive, that are currently invisible to absorption radiography.

X-Ray Absorption Measured in the Resonant Auger Scattering Mode

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hikosaka, Y.; Shigemasa, E.; Kaneyasu, T.

2008-08-15

We report both experimental and theoretical studies on x-ray absorption measured in the resonant Auger scattering mode of gas phase carbon monoxide near the O1s{yields}2{pi} region. Both experiment and theory display a crucial difference between the x-ray absorption profiles obtained in the conventional and resonant scattering modes. Lifetime vibrational interference is the main source of the difference. It is demonstrated that such interference, which arises from a coherent excitation to overlapping intermediate levels, ruins the idea for obtaining x-ray absorption spectra in a lifetime broadening free regime.

High Resolution Spectroscopy of X-ray Quasars: Searching for the X-ray Absorption from the Warm-Hot Intergalactic Medium

NASA Technical Reports Server (NTRS)

Fang, Taotao; Canizares, Claude R.; Marshall, Herman L.

2004-01-01

We present a survey of six low to moderate redshift quasars with Chandra and XMM-Newton. The primary goal is to search for the narrow X-ray absorption lines produced by highly ionized metals in the Warm-Hot Intergalactic Medium. All the X-ray spectra can be well fitted by a power law with neutral hydrogen absorption. Only one feature is detected at above 3-sigma level in all the spectra, which is consistent with statistic fluctuation. We discuss the implications in our understanding of the baryon content of the universe. We also discuss the implication of the non-detection of the local (z approx. 0) X-ray absorption.

Measurement of absolute regional lung air volumes from near-field x-ray speckles.

PubMed

Leong, Andrew F T; Paganin, David M; Hooper, Stuart B; Siew, Melissa L; Kitchen, Marcus J

2013-11-18

Propagation-based phase contrast x-ray (PBX) imaging yields high contrast images of the lung where airways that overlap in projection coherently scatter the x-rays, giving rise to a speckled intensity due to interference effects. Our previous works have shown that total and regional changes in lung air volumes can be accurately measured from two-dimensional (2D) absorption or phase contrast images when the subject is immersed in a water-filled container. In this paper we demonstrate how the phase contrast speckle patterns can be used to directly measure absolute regional lung air volumes from 2D PBX images without the need for a water-filled container. We justify this technique analytically and via simulation using the transport-of-intensity equation and calibrate the technique using our existing methods for measuring lung air volume. Finally, we show the full capabilities of this technique for measuring regional differences in lung aeration.

A nearly on-axis spectroscopic system for simultaneously measuring UV-visible absorption and X-ray diffraction in the SPring-8 structural genomics beamline.

PubMed

Sakaguchi, Miyuki; Kimura, Tetsunari; Nishida, Takuma; Tosha, Takehiko; Sugimoto, Hiroshi; Yamaguchi, Yoshihiro; Yanagisawa, Sachiko; Ueno, Go; Murakami, Hironori; Ago, Hideo; Yamamoto, Masaki; Ogura, Takashi; Shiro, Yoshitsugu; Kubo, Minoru

2016-01-01

UV-visible absorption spectroscopy is useful for probing the electronic and structural changes of protein active sites, and thus the on-line combination of X-ray diffraction and spectroscopic analysis is increasingly being applied. Herein, a novel absorption spectrometer was developed at SPring-8 BL26B2 with a nearly on-axis geometry between the X-ray and optical axes. A small prism mirror was placed near the X-ray beamstop to pass the light only 2° off the X-ray beam, enabling spectroscopic analysis of the X-ray-exposed volume of a crystal during X-ray diffraction data collection. The spectrometer was applied to NO reductase, a heme enzyme that catalyzes NO reduction to N2O. Radiation damage to the heme was monitored in real time during X-ray irradiation by evaluating the absorption spectral changes. Moreover, NO binding to the heme was probed via caged NO photolysis with UV light, demonstrating the extended capability of the spectrometer for intermediate analysis.

Optical spectroscopies diagnose cancer

NASA Astrophysics Data System (ADS)

Alfano, Robert R.; Das, Bidyut B.; Glassman, Wenling S.; Pradhan, Asima; Tang, Gui C.

1992-02-01

Today's medical professional is looking beyond the conventional procedures of X-rays, nuclear radiation, magnetic resonance, chemical analysis, and ultrasound to diagnose diseases ranging from cancer to heart ailments. In view of the possible dangerous side effects of X-rays and nuclear radiation, a need exists for novel techniques in disease detection that can either eliminate or reduce their use in examinations. For more than half a century, fluorescence, absorption, and light scattering spectroscopies have been widely used as probes to acquire fundamental knowledge about various physical, chemical, and biological processes. Light may offer alternatives to X-rays and nuclear approaches, and in some cases is non-invasive. Optical spectroscopy and laser technology may offer techniques for the detection and characterization of physical and chemical changes that occur in diseased tissue on a microscopic level.

Joint reconstruction of x-ray fluorescence and transmission tomography

PubMed Central

Di, Zichao Wendy; Chen, Si; Hong, Young Pyo; Jacobsen, Chris; Leyffer, Sven; Wild, Stefan M.

2017-01-01

X-ray fluorescence tomography is based on the detection of fluorescence x-ray photons produced following x-ray absorption while a specimen is rotated; it provides information on the 3D distribution of selected elements within a sample. One limitation in the quality of sample recovery is the separation of elemental signals due to the finite energy resolution of the detector. Another limitation is the effect of self-absorption, which can lead to inaccurate results with dense samples. To recover a higher quality elemental map, we combine x-ray fluorescence detection with a second data modality: conventional x-ray transmission tomography using absorption. By using these combined signals in a nonlinear optimization-based approach, we demonstrate the benefit of our algorithm on real experimental data and obtain an improved quantitative reconstruction of the spatial distribution of dominant elements in the sample. Compared with single-modality inversion based on x-ray fluorescence alone, this joint inversion approach reduces ill-posedness and should result in improved elemental quantification and better correction of self-absorption. PMID:28788848

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hopkins, Rebecca J.; Lewis, K.; Desyaterik, Yury

Aerosols generated from burning different plant fuels were characterized to determine relationships between chemical, optical and physical properties. Single scattering albedo ({omega}) and Angstrom absorption coefficients ({alpha}{sub ap}) were measured using a photoacoustic technique combined with a reciprocal nephelometer. Carbon-to-oxygen atomic ratios, sp{sup 2} hybridization, elemental composition and morphology of individual particles were measured using scanning transmission X-ray microscopy coupled with near-edge X-ray absorption fine structure spectroscopy (STXM/NEXAFS) and scanning electron microscopy with energy dispersion of X-rays (SEM/EDX). Particles were grouped into three categories based on sp2 hybridization and chemical composition. Measured {omega} (0.4-1.0 at 405 nm) and {alpha}{sub ap}more » (1.0-3.5) values displayed a fuel dependence. The category with sp{sup 2} hybridization >80% had values of {omega} (<0.5) and {alpha}{sub ap} ({approx}1.25) characteristic of light absorbing soot. Other categories with lower sp2 hybridization (20 to 60%) exhibited higher {omega} (>0.8) and {alpha}{sub ap} (1.0 to 3.5) values, indicating increased absorption spectral selectivity.« less

Soft X-ray Absorption Edges in LMXBs

NASA Technical Reports Server (NTRS)

2004-01-01

The XMM observation of LMC X-2 is part of our program to study X-ray absorption in the interstellar medium (ISM). This program includes a variety of bright X-ray binaries in the Galaxy as well as the Magellanic Clouds (LMC and SMC). LMC X-2 is located near the heart of the LMC. Its very soft X-ray spectrum is used to determine abundance and ionization fractions of neutral and lowly ionized oxygen of the ISM in the LMC. The RGS spectrum so far allowed us to determine the O-edge value to be for atomic O, the EW of O-I in the ls-2p resonance absorption line, and the same for O-II. The current study is still ongoing in conjunction with other low absorption sources like Sco X-1 and the recently observed X-ray binary 4U 1957+11.

Multimodality hard-x-ray imaging of a chromosome with nanoscale spatial resolution

DOE PAGES

Yan, Hanfei; Nazaretski, Evgeny; Lauer, Kenneth R.; ...

2016-02-05

Here, we developed a scanning hard x-ray microscope using a new class of x-ray nano-focusing optic called a multilayer Laue lens and imaged a chromosome with nanoscale spatial resolution. The combination of the hard x-ray's superior penetration power, high sensitivity to elemental composition, high spatial-resolution and quantitative analysis creates a unique tool with capabilities that other microscopy techniques cannot provide. Using this microscope, we simultaneously obtained absorption-, phase-, and fluorescence-contrast images of Pt-stained human chromosome samples. The high spatial-resolution of the microscope and its multi-modality imaging capabilities enabled us to observe the internal ultra-structures of a thick chromosome without sectioningmore » it.« less

Multimodality hard-x-ray imaging of a chromosome with nanoscale spatial resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yan, Hanfei; Nazaretski, Evgeny; Lauer, Kenneth R.

Here, we developed a scanning hard x-ray microscope using a new class of x-ray nano-focusing optic called a multilayer Laue lens and imaged a chromosome with nanoscale spatial resolution. The combination of the hard x-ray's superior penetration power, high sensitivity to elemental composition, high spatial-resolution and quantitative analysis creates a unique tool with capabilities that other microscopy techniques cannot provide. Using this microscope, we simultaneously obtained absorption-, phase-, and fluorescence-contrast images of Pt-stained human chromosome samples. The high spatial-resolution of the microscope and its multi-modality imaging capabilities enabled us to observe the internal ultra-structures of a thick chromosome without sectioningmore » it.« less

Interlaced X-ray diffraction computed tomography

PubMed Central

Vamvakeros, Antonios; Jacques, Simon D. M.; Di Michiel, Marco; Senecal, Pierre; Middelkoop, Vesna; Cernik, Robert J.; Beale, Andrew M.

2016-01-01

An X-ray diffraction computed tomography data-collection strategy that allows, post experiment, a choice between temporal and spatial resolution is reported. This strategy enables time-resolved studies on comparatively short timescales, or alternatively allows for improved spatial resolution if the system under study, or components within it, appear to be unchanging. The application of the method for studying an Mn–Na–W/SiO2 fixed-bed reactor in situ is demonstrated. Additionally, the opportunities to improve the data-collection strategy further, enabling post-collection tuning between statistical, temporal and spatial resolutions, are discussed. In principle, the interlaced scanning approach can also be applied to other pencil-beam tomographic techniques, like X-ray fluorescence computed tomography, X-ray absorption fine structure computed tomography, pair distribution function computed tomography and tomographic scanning transmission X-ray microscopy. PMID:27047305

Structural and elemental changes in glioblastoma cells in situ: complementary imaging with high resolution visible light- and X-ray microscopy

DOE PAGES

Ducic, Tanja; Paunesku, Tatjana; Chen, Si; ...

2016-12-09

The glioblastoma (GBM) is characterized by a short median survival and an almost 100% tumor related mortality. GBM cells exhibit highly invasive behavior whose mechanisms are not yet fully understood. The present study explores application of X-ray and visible light microscopy to display the elemental and structural images of cells from 3 patient derived GMB samples and an established GMB cell line. Slight differences in elemental concentrations, in actin cytoskeleton organization and cell morphology were noted between all cells types by X-ray fluorescence and full field soft X-ray microscopy, as well as the Structured Illumination Super-resolution Microscope (SIM). Different samplemore » preparation approaches were used to match each imaging technique. While preparation for SIM included cell fixation and staining, intact frozen hydrated cells were used for the trace element imaging by hard X-ray fluorescence and exploration of the structural features by soft X-ray absorption tomography. In conclusion, each technique documented differences between samples with regard to morphology and elemental composition and underscored the importance of use of multiple patient derived samples for detailed GBM study.« less

Structural and elemental changes in glioblastoma cells in situ: complementary imaging with high resolution visible light- and X-ray microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ducic, Tanja; Paunesku, Tatjana; Chen, Si

The glioblastoma (GBM) is characterized by a short median survival and an almost 100% tumor related mortality. GBM cells exhibit highly invasive behavior whose mechanisms are not yet fully understood. The present study explores application of X-ray and visible light microscopy to display the elemental and structural images of cells from 3 patient derived GMB samples and an established GMB cell line. Slight differences in elemental concentrations, in actin cytoskeleton organization and cell morphology were noted between all cells types by X-ray fluorescence and full field soft X-ray microscopy, as well as the Structured Illumination Super-resolution Microscope (SIM). Different samplemore » preparation approaches were used to match each imaging technique. While preparation for SIM included cell fixation and staining, intact frozen hydrated cells were used for the trace element imaging by hard X-ray fluorescence and exploration of the structural features by soft X-ray absorption tomography. In conclusion, each technique documented differences between samples with regard to morphology and elemental composition and underscored the importance of use of multiple patient derived samples for detailed GBM study.« less

Real-time phase-contrast x-ray imaging: a new technique for the study of animal form and function

PubMed Central

Socha, John J; Westneat, Mark W; Harrison, Jon F; Waters, James S; Lee, Wah-Keat

2007-01-01

Background Despite advances in imaging techniques, real-time visualization of the structure and dynamics of tissues and organs inside small living animals has remained elusive. Recently, we have been using synchrotron x-rays to visualize the internal anatomy of millimeter-sized opaque, living animals. This technique takes advantage of partially-coherent x-rays and diffraction to enable clear visualization of internal soft tissue not viewable via conventional absorption radiography. However, because higher quality images require greater x-ray fluxes, there exists an inherent tradeoff between image quality and tissue damage. Results We evaluated the tradeoff between image quality and harm to the animal by determining the impact of targeted synchrotron x-rays on insect physiology, behavior and survival. Using 25 keV x-rays at a flux density of 80 μW/mm-2, high quality video-rate images can be obtained without major detrimental effects on the insects for multiple minutes, a duration sufficient for many physiological studies. At this setting, insects do not heat up. Additionally, we demonstrate the range of uses of synchrotron phase-contrast imaging by showing high-resolution images of internal anatomy and observations of labeled food movement during ingestion and digestion. Conclusion Synchrotron x-ray phase contrast imaging has the potential to revolutionize the study of physiology and internal biomechanics in small animals. This is the only generally applicable technique that has the necessary spatial and temporal resolutions, penetrating power, and sensitivity to soft tissue that is required to visualize the internal physiology of living animals on the scale from millimeters to microns. PMID:17331247

Photochemically Generated Thiyl Free Radicals Observed by X-ray Absorption Spectroscopy

DOE PAGES

Sneeden, Eileen Y.; Hackett, Mark J.; Cotelesage, Julien J. H.; ...

2017-07-27

Sulfur-based thiyl radicals are known to be involved in a wide range of chemical and biological processes, but they are often highly reactive, which makes them difficult to observe directly. We report herein X-ray absorption spectra and analysis that support the direct observation of two different thiyl species generated photochemically by X-ray irradiation. The thiyl radical sulfur K-edge X-ray absorption spectra of both species are characterized by a uniquely low energy transition at about 2465 eV, which occurs at a lower energy than any previously observed feature at the sulfur K-edge and corresponds to a 1s → 3p transition tomore » the singly occupied molecular orbital of the free radical. In conclusion, our results constitute the first observation of substantial levels of thiyl radicals generated by X-ray irradiation and detected by sulfur K-edge X-ray absorption spectroscopy.« less

Small scale H I structure and the soft X-ray background

NASA Technical Reports Server (NTRS)

Jahoda, K.; Mccammon, D.; Lockman, F. J.

1986-01-01

The observed anticorrelation between diffuse soft X-ray flux and H I column density has been explained as absorption of soft X-rays produced in a hot galactic halo, assuming that the neutral interstellar material is sufficiently clumped to reduce the soft X-ray absorption cross section by a factor of two to three. A 21 cm emission line study of H I column density variations at intermediate and high galactic latitudes to 10' spatial resolution has been done. The results confirm conclusions from preliminary work at coarser resolution, and in combination with other data appear to rule out the hypothesis that clumping of neutral interstellar matter on any angular scale significantly reduces X-ray absorption cross sections in the 0.13 - 0.28 keV energy range. It is concluded therefore that the observed anticorrelation is not primarily a consequence of absorption of soft X-rays produced in a hot galactic halo.

Experimental and theoretical comparison of the O K-edge nonresonant inelastic X-ray scattering and X-ray absorption spectra of NaReO4.

PubMed

Bradley, Joseph A; Yang, Ping; Batista, Enrique R; Boland, Kevin S; Burns, Carol J; Clark, David L; Conradson, Steven D; Kozimor, Stosh A; Martin, Richard L; Seidler, Gerald T; Scott, Brian L; Shuh, David K; Tyliszczak, Tolek; Wilkerson, Marianne P; Wolfsberg, Laura E

2010-10-06

Accurate X-ray absorption spectra (XAS) of first row atoms, e.g., O, are notoriously difficult to obtain due to the extreme sensitivity of the measurement to surface contamination, self-absorption, and saturation affects. Herein, we describe a comprehensive approach for determining reliable O K-edge XAS data for ReO(4)(1-) and provide methodology for obtaining trustworthy and quantitative data on nonconducting molecular systems, even in the presence of surface contamination. This involves comparing spectra measured by nonresonant inelastic X-ray scattering (NRIXS), a bulk-sensitive technique that is not prone to X-ray self-absorption and provides exact peak intensities, with XAS spectra obtained by three different detection modes, namely total electron yield (TEY), fluorescence yield (FY), and scanning transmission X-ray microscopy (STXM). For ReO(4)(1-), TEY measurements were heavily influenced by surface contamination, while the FY and STXM data agree well with the bulk NRIXS analysis. These spectra all showed two intense pre-edge features indicative of the covalent interaction between the Re 5d and O 2p orbitals. Density functional theory calculations were used to assign these two peaks as O 1s excitations to the e and t(2) molecular orbitals that result from Re 5d and O 2p covalent mixing in T(d) symmetry. Electronic structure calculations were used to determine the amount of O 2p character (%) in these molecular orbitals. Time dependent-density functional theory (TD-DFT) was also used to calculate the energies and intensities of the pre-edge transitions. Overall, under these experimental conditions, this analysis suggests that NRIXS, STXM, and FY operate cooperatively, providing a sound basis for validation of bulk-like excitation spectra and, in combination with electronic structure calculations, suggest that NaReO(4) may serve as a well-defined O K-edge energy and intensity standard for future O K-edge XAS studies.

Disentangling atomic-layer-specific x-ray absorption spectra by Auger electron diffraction spectroscopy

NASA Astrophysics Data System (ADS)

Matsui, Fumihiko; Matsushita, Tomohiro; Kato, Yukako; Hashimoto, Mie; Daimon, Hiroshi

2009-11-01

In order to investigate the electronic and magnetic structures of each atomic layer at subsurface, we have proposed a new method, Auger electron diffraction spectroscopy, which is the combination of x-ray absorption spectroscopy (XAS) and Auger electron diffraction (AED) techniques. We have measured a series of Ni LMM AED patterns of the Ni film grown on Cu(001) surface for various thicknesses. Then we deduced a set of atomic-layer-specific AED patterns in a numerical way. Furthermore, we developed an algorithm to disentangle XANES spectra from different atomic layers using these atomic-layer-specific AED patterns. Surface and subsurface core level shift were determined for each atomic layer.

Grazing incidence X-ray absorption characterization of amorphous Zn-Sn-O thin film

NASA Astrophysics Data System (ADS)

Moffitt, S. L.; Ma, Q.; Buchholz, D. B.; Chang, R. P. H.; Bedzyk, M. J.; Mason, T. O.

2016-05-01

We report a surface structure study of an amorphous Zn-Sn-O (a-ZTO) transparent conducting film using the grazing incidence X-ray absorption spectroscopy technique. By setting the measuring angles far below the critical angle at which the total external reflection occurs, the details of the surface structure of a film or bulk can be successfully accessed. The results show that unlike in the film where Zn is severely under coordinated (N < 4), it is fully coordinated (N = 4) near the surface while the coordination number around Sn is slightly smaller near the surface than in the film. Despite a 30% Zn doping, the local structure in the film is rutile-like.

SYNCHROTRON RADIATION, FREE ELECTRON LASER, APPLICATION OF NUCLEAR TECHNOLOGY, ETC.: A new cell for X-ray absorption spectroscopy study under high pressure

NASA Astrophysics Data System (ADS)

Zheng, Li-Rong; Che, Rong-Zheng; Liu, Jing; Du, Yong-Hua; Zhou, Ying-Li; Hu, Tian-Dou

2009-08-01

X-ray absorption fine structure (XAFS) spectroscopy is a powerful technique for the investigation of the local environment around selected atoms in condensed matter. XAFS under pressure is an important method for the synchrotron source. We design a cell for a high pressure XAFS experiment. Sintered boron carbide is used as the anvils of this high pressure cell in order to obtain a full XAFS spectrum free from diffraction peaks. In addition, a hydraulic pump was adopted to make in-suit pressure modulation. High quality XAFS spectra of ZrH2 under high pressure (up to 13 GPa) were obtained by this cell.

High-pressure studies on nanocrystalline borderline Co1-xFexS2 (x = 0.4 and 0.5) using Mössbauer spectroscopic and electrical resistivity techniques up to 8 GPa

NASA Astrophysics Data System (ADS)

Chandra, Usha; Sharma, Pooja; Parthasarathy, G.

2016-12-01

Like bulk, Co1-xFexS2 nanoparticles also display an anomaly at x = 0.5. The borderline contiguous Co1-xFexS2 (x = 0.4 and 0.5) nanoparticles were synthesized with colloidal method and characterized for pyrite structure using various techniques, viz., X-ray diffraction, energy dispersive X-ray analysis (EDAX), S K-edge X-ray absorption near edge spectra, transmission electron microscopy (TEM) and Fourier transformed infra-red spectroscopy. The report presents the effect of high pressure on the borderline compositions using the Mössbauer spectroscopic and electrical resistivity techniques. Magnetic measurements on the system showed drastic lowering of Tc due to nanosize of the particles. With increased pressure, quadrupole splitting showed an expected trend of increase to attain a peak representing a second-order phase transition between 4 and 5 GPa for both the compositions. The pressure coefficient of electrical resistivity varied from -0.02 GPa to -0.06 GPa across transition pressure indicating a sluggish nature of transition. This is the first report of pressure effect on nanosized borderline compositions.

Time-resolved measurements of supersonic fuel sprays using synchrotron X-rays.

PubMed

Powell, C F; Yue, Y; Poola, R; Wang, J

2000-11-01

A time-resolved radiographic technique has been developed for probing the fuel distribution close to the nozzle of a high-pressure single-hole diesel injector. The measurement was made using X-ray absorption of monochromatic synchrotron-generated radiation, allowing quantitative determination of the fuel distribution in this optically impenetrable region with a time resolution of better than 1 micros. These quantitative measurements constitute the most detailed near-nozzle study of a fuel spray to date.

Atomistic simulation and XAS investigation of Mn induced defects in Bi{sub 12}TiO{sub 20}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rezende, Marcos V dos S.; Santos, Denise J.; Jackson, Robert A.

2016-06-15

This work reports an investigation of the valence and site occupancy of Mn dopants in Bi{sub 12}TiO{sub 20} (BTO: Mn) host using X-ray Absorption (XAS) and atomistic simulation techniques based on energy minimisation. X-ray Absorption Near Edge Structure (XANES) at the Mn K-edges gave typical results for Mn ions with mixed valences of 3+ and 4+. Extended X-ray Absorption Fine Structure (EXAFS) results indicated that Mn ions are probably substituted at Ti sites. Atomistic simulation was performed assuming the incorporation of Mn{sup 2+}, Mn{sup 3+} and Mn{sup 4+} ions at either Bi{sup 3+} or Ti{sup 4+} sites, and the resultsmore » were compared to XANES and EXAFS measurements. Electrical conductivity for pure and doped samples was used to evaluate the consistency of the proposed model. - Graphical abstract: The structure of Bi{sub 12}TiO{sub 20} (BTO). Display Omitted - Highlights: • Pure and Mn-doped Bi{sub 12}TiO{sub 20} samples were studied by experimental techniques combined with atomistic simulation. • Good agreement between experimental and simulation results was obtained. • XANES results suggest a mixture of 3+ and 4+ valences for Mn, occupying the Ti4+ site in both cases. • Charge compensation by holes is most energetically favoured, explaining the enhancement observed in AC dark conductivity.« less

Nondestructive Evaluation of Advanced Materials with X-ray Phase Mapping

NASA Technical Reports Server (NTRS)

Hu, Zhengwei

2005-01-01

X-ray radiation has been widely used for imaging applications since Rontgen first discovered X-rays over a century ago. Its large penetration depth makes it ideal for the nondestructive visualization of the internal structure and/or defects of materials unobtainable otherwise. Currently used nondestructive evaluation (NDE) tools, X-ray radiography and tomography, are absorption-based, and work well in heavy-element materials where density or composition variations due to internal structure or defects are high enough to produce appreciable absorption contrast. However, in many cases where materials are light-weight and/or composites that have similar mass absorption coefficients, the conventional absorption-based X-ray methods for NDE become less useful. Indeed, the light-weight and ultra-high-strength requirements for the most advanced materials used or developed for current flight mission and future space exploration pose a great challenge to the standard NDE tools in that the absorption contrast arising from the internal structure of these materials is often too weak to be resolved. In this presentation, a solution to the problem, the use of phase information of X-rays for phase contrast X-ray imaging, will be discussed, along with a comparison between the absorption-based and phase-contrast imaging methods. Latest results on phase contrast X-ray imaging of lightweight Space Shuttle foam in 2D and 3D will be presented, demonstrating new opportunities to solve the challenging issues encountered in advanced materials development and processing.

Anionic and cationic redox and interfaces in batteries: Advances from soft X-ray absorption spectroscopy to resonant inelastic scattering

NASA Astrophysics Data System (ADS)

Yang, Wanli; Devereaux, Thomas P.

2018-06-01

Recent advances in battery science and technology have triggered both the challenges and opportunities on studying the materials and interfaces in batteries. Here, we review the recent demonstrations of soft X-ray spectroscopy for studying the interfaces and electrode materials. The focus of this review is on the recently developed mapping of resonant inelastic X-ray scattering (mRIXS) as a powerful probe of battery chemistry with superior sensitivity. Six different channels of soft X-ray absorption spectroscopy (sXAS) are introduced for different experimental purposes. Although conventional sXAS channels remain effective tools for quantitative analysis of the transition-metal states and surface chemistry, we elaborate the limitations of sXAS in both cationic and anionic redox studies. Particularly, based on experimental findings in various electrodes, we show that sXAS is unreliable for studying oxygen redox. We then demonstrate the mRIXS as a reliable technique for fingerprinting oxygen redox and summarize several crucial observations. We conclude that mRIXS is the tool-of-choice to study both the practical issue on reversibility of oxygen redox and the fundamental nature of bulk oxygen states. We hope this review clarifies the popular misunderstanding on oxygen sXAS results of oxide electrodes, and establishes a reliable technique for detecting oxygen redox through mRIXS.

THE BLAZAR EMISSION ENVIRONMENT: INSIGHT FROM SOFT X-RAY ABSORPTION

DOE Office of Scientific and Technical Information (OSTI.GOV)

Furniss, A.; Williams, D. A.; Fumagalli, M.

Collecting experimental insight into the relativistic particle populations and emission mechanisms at work within TeV-emitting blazar jets, which are spatially unresolvable in most bands and have strong beaming factors, is a daunting task. New observational information has the potential to lead to major strides in understanding the acceleration site parameters. Detection of molecular carbon monoxide (CO) in TeV emitting blazars, however, implies the existence of intrinsic gas, a connection often found in photo-dissociated region models and numerical simulations. The existence of intrinsic gas within a blazar could provide a target photon field for Compton up-scattering of photons to TeV energiesmore » by relativistic particles. We investigate the possible existence of intrinsic gas within the three TeV emitting blazars RGB J0710+591, W Comae, and 1ES 1959+650 which have measurements or upper limits on molecular CO line luminosity using an independent technique that is based on the spectral analysis of soft X-rays. Evidence for X-ray absorption by additional gas beyond that measured within the Milky Way is searched for in Swift X-ray Telescope (XRT) data between 0.3 and 10 keV. Without complementary information from another measurement, additional absorption could be misinterpreted as an intrinsically curved X-ray spectrum since both models can frequently fit the soft X-ray data. After breaking this degeneracy, we do not find evidence for intrinsically curved spectra for any of the three blazars. Moreover, no evidence for intrinsic gas is evident for RGB J0710+591 and W Comae, while the 1ES 1959+650 XRT data support the existence of intrinsic gas with a column density of {approx}1 Multiplication-Sign 10{sup 21} cm{sup -2}.« less

X-Ray Attenuation and Absorption for Materials of Dosimetric Interest

National Institute of Standards and Technology Data Gateway

SRD 126 X-Ray Attenuation and Absorption for Materials of Dosimetric Interest (Web, free access)   Tables and graphs of the photon mass attenuation coefficient and the mass energy-absorption coefficient are presented for all of the elements Z = 1 to 92, and for 48 compounds and mixtures of radiological interest. The tables cover energies of the photon (x-ray, gamma ray, bremsstrahlung) from 1 keV to 20 MeV.

Analysis of field of view limited by a multi-line X-ray source and its improvement for grating interferometry.

PubMed

Du, Yang; Huang, Jianheng; Lin, Danying; Niu, Hanben

2012-08-01

X-ray phase-contrast imaging based on grating interferometry is a technique with the potential to provide absorption, differential phase contrast, and dark-field signals simultaneously. The multi-line X-ray source used recently in grating interferometry has the advantage of high-energy X-rays for imaging of thick samples for most clinical and industrial investigations. However, it has a drawback of limited field of view (FOV), because of the axial extension of the X-ray emission area. In this paper, we analyze the effects of axial extension of the multi-line X-ray source on the FOV and its improvement in terms of Fresnel diffraction theory. Computer simulation results show that the FOV limitation can be overcome by use of an alternative X-ray tube with a specially designed multi-step anode. The FOV of this newly designed X-ray source can be approximately four times larger than that of the multi-line X-ray source in the same emission area. This might be beneficial for the applications of X-ray phase contrast imaging in materials science, biology, medicine, and industry.

X-ray scanning of overhead aurorae from rockets

NASA Technical Reports Server (NTRS)

Barcus, J. R.; Goldberg, R. A.; Gesell, L. H.

1981-01-01

Two Nike Tomahawk rocket payloads were launched into energetic auroral events in September, 1976 to investigate the structure of these events, as well as their effects on the atmosphere. X-ray scintillation detectors with energy discrimination in four ranges were used to measure the deposition of bremsstrahlung produced X-rays within the stratosphere and mesosphere. Iterative computer techniques were used to reconstruct X-ray source maps at 100 km, taking atmospheric absorption effects into account. Payload 18.178 was launched on September 21st into an aurora having two distinct azimuthal regions of optical brightness. The X-ray scanner detected the same features, and overlays of the X-ray source maps on all-sky photographs showed spatial coincidence of the X-ray with optical features at the lower energies (below 40 keV). Payload 18.179 was launched September 23rd into an aurora with a more diffuse character. The optical structure did not coincide as well with the measured X-ray structure. There was also an indication of a two-component spectrum for each event, with the hard component originating in the more diffuse, optically faint regions.

Full-Field Calcium K-Edge X-ray Absorption Near-Edge Structure Spectroscopy on Cortical Bone at the Micron-Scale: Polarization Effects Reveal Mineral Orientation.

PubMed

Hesse, Bernhard; Salome, Murielle; Castillo-Michel, Hiram; Cotte, Marine; Fayard, Barbara; Sahle, Christoph J; De Nolf, Wout; Hradilova, Jana; Masic, Admir; Kanngießer, Birgit; Bohner, Marc; Varga, Peter; Raum, Kay; Schrof, Susanne

2016-04-05

Here, we show results on X-ray absorption near edge structure spectroscopy in both transmission and X-ray fluorescence full-field mode (FF-XANES) at the calcium K-edge on human bone tissue in healthy and diseased conditions and for different tissue maturation stages. We observe that the dominating spectral differences originating from different tissue regions, which are well pronounced in the white line and postedge structures are associated with polarization effects. These polarization effects dominate the spectral variance and must be well understood and modeled before analyzing the very subtle spectral variations related to the bone tissue variations itself. However, these modulations in the fine structure of the spectra can potentially be of high interest to quantify orientations of the apatite crystals in highly structured tissue matrices such as bone. Due to the extremely short wavelengths of X-rays, FF-XANES overcomes the limited spatial resolution of other optical and spectroscopic techniques exploiting visible light. Since the field of view in FF-XANES is rather large the acquisition times for analyzing the same region are short compared to, for example, X-ray diffraction techniques. Our results on the angular absorption dependence were verified by both site-matched polarized Raman spectroscopy, which has been shown to be sensitive to the orientation of bone building blocks and by mathematical simulations of the angular absorbance dependence. As an outlook we further demonstrate the polarization based assessment of calcium-containing crystal orientation and specification of calcium in a beta-tricalcium phosphate (β-Ca3(PO4)2 scaffold implanted into ovine bone. Regarding the use of XANES to assess chemical properties of Ca in human bone tissue our data suggest that neither the anatomical site (tibia vs jaw) nor pathology (healthy vs necrotic jaw bone tissue) affected the averaged spectral shape of the XANES spectra.

Exploring actinide materials through synchrotron radiation techniques.

PubMed

Shi, Wei-Qun; Yuan, Li-Yong; Wang, Cong-Zhi; Wang, Lin; Mei, Lei; Xiao, Cheng-Liang; Zhang, Li; Li, Zi-Jie; Zhao, Yu-Liang; Chai, Zhi-Fang

2014-12-10

Synchrotron radiation (SR) based techniques have been utilized with increasing frequency in the past decade to explore the brilliant and challenging sciences of actinide-based materials. This trend is partially driven by the basic needs for multi-scale actinide speciation and bonding information and also the realistic needs for nuclear energy research. In this review, recent research progresses on actinide related materials by means of various SR techniques were selectively highlighted and summarized, with the emphasis on X-ray absorption spectroscopy, X-ray diffraction and scattering spectroscopy, which are powerful tools to characterize actinide materials. In addition, advanced SR techniques for exploring future advanced nuclear fuel cycles dealing with actinides are illustrated as well. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A multiple technique approach to the analysis of urinary calculi.

PubMed

Rodgers, A L; Nassimbeni, L R; Mulder, K J

1982-01-01

10 urinary calculi have been qualitatively and quantitatively analysed using X-ray diffraction, infra-red, scanning electron microscopy, X-ray fluorescence, atomic absorption and density gradient procedures. Constituents and compositional features which often go undetected due to limitations in the particular analytical procedure being used, have been identified and a detailed picture of each stone's composition and structure has been obtained. In all cases at least two components were detected suggesting that the multiple technique approach might cast some doubt as to the existence of "pure" stones. Evidence for a continuous, non-sequential deposition mechanism has been detected. In addition, the usefulness of each technique in the analysis of urinary stones has been assessed and the multiple technique approach has been evaluated as a whole.

Structural, optical and enhanced power filtering application of PEG capped Zn1-xCoxS quantum dots

NASA Astrophysics Data System (ADS)

Vineeshkumar, T. V.; Prasanth, S.; Pragash, R.; Unnikrishnan, N. V.; Sudarsanakumar, C.

2018-04-01

Zn1-xCoxS (x= 0.05, 0.1, 0.15 and 0.2) quantum dots were synthesized successfully using co precipitation technique in polyethylene glycol (PEG) matrix. The PEG acted as a capping agent as well as a reducing agent. The structural and optical properties of the samples were studied by x-ray diffraction (XRD), TEM analysis and UV-Visible absorption. Nonlinear optical properties were measured using open aperture z-scan technique, employing frequency doubled (532 nm) pumping sources.

Table-top phase-contrast imaging employing photon-counting detectors towards mammographic applications

NASA Astrophysics Data System (ADS)

Palma, K. D.; Pichotka, M.; Hasn, S.; Granja, C.

2017-02-01

In mammography the difficult task to detect microcalcifications (≈ 100 μm) and low contrast structures in the breast has been a topic of interest from its beginnings. The possibility to improve the image quality requires the effort to employ novel X-ray imaging techniques, such as phase-contrast, and high resolution detectors. Phase-contrast techniques are promising tools for medical diagnosis because they provide additional and complementary information to traditional absorption-based X-ray imaging methods. In this work a Hamamatsu microfocus X-ray source with tungsten anode and a photon counting detector (Timepix operated in Medipix mode) was used. A significant improvement in the detection of phase-effects using Medipix detector was observed in comparison to an standard flat-panel detector. An optimization of geometrical parameters reveals the dependency on the X-ray propagation path and the small angle deviation. The quantification of these effects was achieved taking into account the image noise, contrast, spatial resolution of the phase-enhancement, absorbed dose, and energy dependence.

CuInGaSe{sub 2} nanoparticles by pulsed laser ablation in liquid medium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mendivil, M.I.; García, L.V.; Krishnan, B.

2015-12-15

Highlights: • CIGS nanocolloids were synthesized using PLAL technique. • Characterized their morphology, structure, composition and optical properties. • Morphologies were dependent on ablation wavelength and liquid medium. • Optical absorption and bandgap of these nanocolloids were tunable. - Abstract: Pulsed laser ablation in liquid medium (PLALM) is a nanofabrication technique to produce complex nanostructures. CuInGaSe{sub 2} (CIGS) is an alloy with applications in photovoltaic industry. In this work, we studied the effects of laser ablation wavelength, energy fluence and liquid medium on the properties of the CIGS nanoparticles synthesized by PLALM. The nanoparticles obtained were analyzed by transmission electronmore » microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), selected area electron diffraction (SAED), X-ray photoelectron spectroscopy (XPS) and UV–vis absorption spectroscopy. XPS results confirmed the chemical states and composition of the ablated products. TEM analysis showed different morphologies for the nanomaterials obtained in different liquid media and ablation wavelengths. The optical properties for these CIGS nanocolloids were analyzed using UV–vis absorption spectroscopy. The results demonstrated the use of PLALM as a useful synthesis technique for nanoparticles of quaternary photovoltaic materials.« less

Quantification of rapid environmental redox processes with quick-scanning x-ray absorption spectroscopy (Q-XAS)

PubMed Central

Ginder-Vogel, Matthew; Landrot, Gautier; Fischel, Jason S.; Sparks, Donald L.

2009-01-01

Quantification of the initial rates of environmental reactions at the mineral/water interface is a fundamental prerequisite to determining reaction mechanisms and contaminant transport modeling and predicting environmental risk. Until recently, experimental techniques with adequate time resolution and elemental sensitivity to measure initial rates of the wide variety of environmental reactions were quite limited. Techniques such as electron paramagnetic resonance and Fourier transform infrared spectroscopies suffer from limited elemental specificity and poor sensitivity to inorganic elements, respectively. Ex situ analysis of batch and stirred-flow systems provides high elemental sensitivity; however, their time resolution is inadequate to characterize rapid environmental reactions. Here we apply quick-scanning x-ray absorption spectroscopy (Q-XAS), at sub-second time-scales, to measure the initial oxidation rate of As(III) to As(V) by hydrous manganese(IV) oxide. Using Q-XAS, As(III) and As(V) concentrations were determined every 0.98 s in batch reactions. The initial apparent As(III) depletion rate constants (t < 30 s) measured with Q-XAS are nearly twice as large as rate constants measured with traditional analytical techniques. Our results demonstrate the importance of developing analytical techniques capable of analyzing environmental reactions on the same time scale as they occur. Given the high sensitivity, elemental specificity, and time resolution of Q-XAS, it has many potential applications. They could include measuring not only redox reactions but also dissolution/precipitation reactions, such as the formation and/or reductive dissolution of Fe(III) (hydr)oxides, solid-phase transformations (i.e., formation of layered-double hydroxide minerals), or almost any other reaction occurring in aqueous media that can be measured using x-ray absorption spectroscopy. PMID:19805269

A highly sensitive x-ray imaging modality for hepatocellular carcinoma detection in vitro

NASA Astrophysics Data System (ADS)

Rand, Danielle; Walsh, Edward G.; Derdak, Zoltan; Wands, Jack R.; Rose-Petruck, Christoph

2015-01-01

Innovations that improve sensitivity and reduce cost are of paramount importance in diagnostic imaging. The novel x-ray imaging modality called spatial frequency heterodyne imaging (SFHI) is based on a linear arrangement of x-ray source, tissue, and x-ray detector, much like that of a conventional x-ray imaging apparatus. However, SFHI rests on a complete paradigm reversal compared to conventional x-ray absorption-based radiology: while scattered x-rays are carefully rejected in absorption-based x-ray radiology to enhance the image contrast, SFHI forms images exclusively from x-rays scattered by the tissue. In this study we use numerical processing to produce x-ray scatter images of hepatocellular carcinoma labeled with a nanoparticle contrast agent. We subsequently compare the sensitivity of SFHI in this application to that of both conventional x-ray imaging and magnetic resonance imaging (MRI). Although SFHI is still in the early stages of its development, our results show that the sensitivity of SFHI is an order of magnitude greater than that of absorption-based x-ray imaging and approximately equal to that of MRI. As x-ray imaging modalities typically have lower installation and service costs compared to MRI, SFHI could become a cost effective alternative to MRI, particularly in areas of the world with inadequate availability of MRI facilities.

Arsenic speciation in sinter mineralization from a hydrothermal channel of El Tatio geothermal field, Chile

NASA Astrophysics Data System (ADS)

Alsina, Marco A.; Zanella, Luciana; Hoel, Cathleen; Pizarro, Gonzalo E.; Gaillard, Jean-François; Pasten, Pablo A.

2014-10-01

El Tatio geothermal field is the principal natural source of arsenic for the Loa River, the main surface water resource in the hyper-arid Atacama Desert (Antofagasta Region, Northern Chile). Prior investigations by bulk X-ray absorption spectroscopy have identified hydrous ferric oxides as the principal arsenic-containing phase in sinter material from El Tatio, suggesting sorption as the main mechanism for arsenic scavenging by the solid phases of these hot spring environments. Here we examine siliceous sinter material sampled from a hydrothermal channel using synchrotron based X-ray micro-probe techniques, including As and Fe Kα X-ray fluorescence (μ-XRF), As K-edge X-ray absorption near edge structure (μ-XANES), and X-ray diffraction (μ-XRD). Least-squares linear fitting of μ-XANES spectra shows that arsenic is predominantly present as arsenate sorbed on hydrous ferric oxides (63% molar proportion), but we also identify nodular arsenide micro-mineralizations (37% molar proportion) similar to loellingite (FeAs2), not previously detected during bulk-scale analysis of the sinter material. Presence of arsenide mineralizations indicates development of anoxic environments on the surface of the siliceous sinter, and suggests a more complex biogeochemistry for arsenic than previously observed for circum-neutral pH brine hot spring environments.

Anomalous small-angle scattering as a way to solve the Babinet principle problem

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boiko, M. E., E-mail: m.e.boiko@mail.ioffe.ru; Sharkov, M. D.; Boiko, A. M.

2013-12-15

X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

Anomalous small-angle scattering as a way to solve the Babinet principle problem

NASA Astrophysics Data System (ADS)

Boiko, M. E.; Sharkov, M. D.; Boiko, A. M.; Bobyl, A. V.

2013-12-01

X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

Near- and Extended-Edge X-Ray-Absorption Fine-Structure Spectroscopy Using Ultrafast Coherent High-Order Harmonic Supercontinua

NASA Astrophysics Data System (ADS)

Popmintchev, Dimitar; Galloway, Benjamin R.; Chen, Ming-Chang; Dollar, Franklin; Mancuso, Christopher A.; Hankla, Amelia; Miaja-Avila, Luis; O'Neil, Galen; Shaw, Justin M.; Fan, Guangyu; Ališauskas, Skirmantas; Andriukaitis, Giedrius; Balčiunas, Tadas; Mücke, Oliver D.; Pugzlys, Audrius; Baltuška, Andrius; Kapteyn, Henry C.; Popmintchev, Tenio; Murnane, Margaret M.

2018-03-01

Recent advances in high-order harmonic generation have made it possible to use a tabletop-scale setup to produce spatially and temporally coherent beams of light with bandwidth spanning 12 octaves, from the ultraviolet up to x-ray photon energies >1.6 keV . Here we demonstrate the use of this light for x-ray-absorption spectroscopy at the K - and L -absorption edges of solids at photon energies near 1 keV. We also report x-ray-absorption spectroscopy in the water window spectral region (284-543 eV) using a high flux high-order harmonic generation x-ray supercontinuum with 109 photons/s in 1% bandwidth, 3 orders of magnitude larger than has previously been possible using tabletop sources. Since this x-ray radiation emerges as a single attosecond-to-femtosecond pulse with peak brightness exceeding 1026 photons/s /mrad2/mm2/1 % bandwidth, these novel coherent x-ray sources are ideal for probing the fastest molecular and materials processes on femtosecond-to-attosecond time scales and picometer length scales.

Joint reconstruction of x-ray fluorescence and transmission tomography

DOE PAGES

Di, Zichao; Chen, Si; Hong, Young Pyo; ...

2017-05-30

X-ray fluorescence tomography is based on the detection of fluorescence x-ray photons produced following x-ray absorption while a specimen is rotated; it provides information on the 3D distribution of selected elements within a sample. One limitation in the quality of sample recovery is the separation of elemental signals due to the finite energy resolution of the detector. Another limitation is the effect of self-absorption, which can lead to inaccurate results with dense samples. To recover a higher quality elemental map, we combine x-ray fluorescence detection with a second data modality: conventional x-ray transmission tomography using absorption. By using these combinedmore » signals in a nonlinear optimization-based approach, we demonstrate the benefit of our algorithm on real experimental data and obtain an improved quantitative reconstruction of the spatial distribution of dominant elements in the sample. Furthermore, compared with single-modality inversion based on x-ray fluorescence alone, this joint inversion approach reduces ill-posedness and should result in improved elemental quantification and better correction of self-absorption.« less

Incorporation of Cadmium and Nickel into Ferrite Spinel Solid Solution: X-ray Diffraction and X-ray Absorption Fine Structure Analyses.

PubMed

Su, Minhua; Liao, Changzhong; Chan, Tingshan; Shih, Kaimin; Xiao, Tangfu; Chen, Diyun; Kong, Lingjun; Song, Gang

2018-01-16

The feasibility of incorporating Cd and Ni in hematite was studied by investigating the interaction mechanism for the formation of Cd x Ni 1-x Fe 2 O 4 solid solutions (CNFs) from CdO, NiO, and α-Fe 2 O 3 . X-ray diffraction results showed that the CNFs crystallized into spinel structures with increasing lattice parameters as the Cd content in the precursors was increased. Cd 2+ ions were found to occupy the tetrahedral sites, as evidenced by Rietveld refinement and extended X-ray absorption fine structure analyses. The incorporation of Cd and Ni into ferrite spinel solid solution strongly relied on the processing parameters. The incorporation of Cd and Ni into the CNFs was greater at high x values (0.7 < x ≤ 1.0) than at low x values (0.0 ≤ x ≤ 0.7). A feasible treatment technique based on the investigated mechanism of CNF formation was developed, involving thermal treatment of waste sludge containing Cd and Ni. Both of these metals in the waste sludge were successfully incorporated into a ferrite spinel solid solution, and the concentrations of leached Cd and Ni from this solid solution were substantially reduced, stabilizing at low levels. This research offers a highly promising approach for treating the Cd and Ni content frequently encountered in electronic waste and its treatment residues.

Local structural and chemical ordering of nanosized Pt3±δCo probed by multiple-scattering x-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Greco, Giorgia; Witkowska, Agnieszka; Principi, Emiliano; Minicucci, Marco; di Cicco, Andrea

2011-04-01

This work reports a detailed investigation of the local structure and chemical disorder of a Pt3±δCo thin film and Pt3±δCo nanoparticles. We have used a combination of techniques including x-ray absorption spectroscopy (XAS), x-ray diffraction (XRD), and high-resolution transmission electron microscopy (TEM). High-quality XAS spectra at the Co K edge and Pt L3 edge have been analyzed using double-edge multiple-scattering data analysis. Structural extended x-ray absorption fine structure (EXAFS) refinements have been performed accounting for the reduction of the coordination numbers and degeneracy of three-atom configurations, resulting from the measured size distribution and stoichiometry. The important effect of chemical ordering on pair and three-atom configurations has been studied using computer simulations based on a simple model accounting for substitutional disorder, defined by an order parameter s. It has been found that individual EXAFS signals related to the minority species (Co) are extremely sensitive to substitutional disorder so their intensities, especially those of the collinear three-atom configurations, can be used as a measure of the ordering level. The thin film has been found to be chemically disordered (s⩽0.4), in agreement with previous estimates. The Pt3±δCo nanoalloy has been found to be partially ordered (s=0.6±0.1) while the local structure around Co atoms is characterized by a higher level of structural disorder as compared to the bulk-like thin film. The robust approach for nanomaterial characterization used in this work combining different techniques can, in principle, be applied for structural refinements of any binary nanocrystalline functional system.

The BALDER Beamline at the MAX IV Laboratory

NASA Astrophysics Data System (ADS)

Klementiev, K.; Norén, K.; Carlson, S.; Sigfridsson Clauss, K. G. V.; Persson, I.

2016-05-01

X-ray absorption spectroscopy (XAS) includes well-established methods to study the local structure around the absorbing element - extended X-ray absorption fine structure (EXAFS), and the effective oxidation number or to quantitatively determine the speciation of an element in a complex matrix - X-ray absorption near-edge structure (XANES). The increased brilliance and intensities available at the new generation of synchrotron light sources makes it possible to study, in-situ and in-operando, much more dilute systems with relevance for natural systems, as well as the micro-scale variability and dynamics of chemical reactions on the millisecond time-scale. The design of the BALDER beamline at the MAX IV Laboratory 3 GeV ring has focused on a high flux of photons in a wide energy range, 2.4-40 keV, where the K-edge is covered for the elements S to La, and the L 3-edge for all elements heavier than Sb. The overall design of the beamline will allow large flexibility in energy range, beam size and data collection time. The other focus of the beamline design is the possibility to perform multi-technique analyses on samples. Development of sample environment requires focus on implementation of auxiliary methods in such a way that techniques like Fourier transform infrared (FTIR) spectroscopy, UV-Raman spectroscopy, X-ray diffraction and/or mass spectrometry can be performed simultaneously as the XAS study. It will be a flexible system where different instruments can be plugged in and out depending on the needs for the particular investigation. Many research areas will benefit from the properties of the wiggler based light source and the capabilities to perform in-situ and in-operando measurements, for example environmental and geochemical sciences, nuclear chemistry, catalysis, materials sciences, and cultural heritage.

Tracking ink composition on Herculaneum papyrus scrolls: quantification and speciation of lead by X-ray based techniques and Monte Carlo simulations.

PubMed

Tack, Pieter; Cotte, Marine; Bauters, Stephen; Brun, Emmanuel; Banerjee, Dipanjan; Bras, Wim; Ferrero, Claudio; Delattre, Daniel; Mocella, Vito; Vincze, Laszlo

2016-02-08

The writing in carbonized Herculaneum scrolls, covered and preserved by the pyroclastic events of the Vesuvius in 79 AD, was recently revealed using X-ray phase-contrast tomography, without the need of unrolling the sensitive scrolls. Unfortunately, some of the text is difficult to read due to the interference of the papyrus fibers crossing the written text vertically and horizontally. Recently, lead was found as an elemental constituent in the writing, rendering the text more clearly readable when monitoring the lead X-ray fluorescence signal. Here, several hypotheses are postulated for the origin and state of lead in the papyrus writing. Multi-scale X-ray fluorescence micro-imaging, Monte Carlo quantification and X-ray absorption microspectroscopy experiments are used to provide additional information on the ink composition, in an attempt to determine the origin of the lead in the Herculaneum scrolls and validate the postulated hypotheses.

High-resolution x-ray tomography using laboratory sources

NASA Astrophysics Data System (ADS)

Tkachuk, Andrei; Feser, Michael; Cui, Hongtao; Duewer, Fred; Chang, Hauyee; Yun, Wenbing

2006-08-01

X-ray computed tomography (XCT) is a powerful nondestructive 3D imaging technique, which enables the visualization of the three dimensional structure of complex, optically opaque samples. High resolution XCT using Fresnel zone plate lenses has been confined in the past to synchrotron radiation centers due to the need for a bright and intense source of x-rays. This confinement severely limits the availability and accessibility of x-ray microscopes and the wide proliferation of this methodology. We are describing a sub-50nm resolution XCT system operating at 8 keV in absorption and Zernike phase contrast mode based on a commercially available laboratory x-ray source. The system utilizes high-efficiency Fresnel zone plates with an outermost zone width of 35 nm and 700 nm structure height resulting in a current spatial resolution better than 50 nm. In addition to the technical description of the system and specifications, we present application examples in the semiconductor field.

Speciation and distribution of copper in a mining soil using multiple synchrotron-based bulk and microscopic techniques.

PubMed

Yang, Jianjun; Liu, Jin; Dynes, James J; Peak, Derek; Regier, Tom; Wang, Jian; Zhu, Shenhai; Shi, Jiyan; Tse, John S

2014-02-01

Molecular-level understanding of soil Cu speciation and distribution assists in management of Cu contamination in mining sites. In this study, one soil sample, collected from a mining site contaminated since 1950s, was characterized complementarily by multiple synchrotron-based bulk and spatially resolved techniques for the speciation and distribution of Cu as well as other related elements (Fe, Ca, Mn, K, Al, and Si). Bulk X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) spectroscopy revealed that soil Cu was predominantly associated with Fe oxides instead of soil organic matter. This agreed with the closest association of Cu to Fe by microscopic X-ray fluorescence (U-XRF) and scanning transmission X-ray microscopy (STXM) nanoanalysis, along with the non-occurrence of photoreduction of soil Cu(II) by quick Cu L3,2-edge XANES spectroscopy (Q-XANES) which often occurs when Cu organic complexes are present. Furthermore, bulk-EXAFS and STXM-coupled Fe L3,2-edge nano-XANES analysis revealed soil Cu adsorbed primarily to Fe(III) oxides by inner-sphere complexation. Additionally, Cu K-edge μ-XANES, L3,2-edge bulk-XANES, and successive Q-XANES results identified the presence of Cu2S rather than radiation-damage artifacts dominant in certain microsites of the mining soil. This study demonstrates the great benefits in use of multiple combined synchrotron-based techniques for comprehensive understanding of Cu speciation in heterogeneous soil matrix, which facilitates our prediction of Cu reactivity and environmental fate in the mining site.

In situ/Operando studies of electrocatalysts using hard X-ray spectroscopy

DOE PAGES

Lassalle-Kaiser, Benedikt; Gul, Sheraz; Kern, Jan; ...

2017-05-02

This review focuses on the use of X-ray absorption and emission spectroscopy techniques using hard X-rays to study electrocatalysts under in situ/operando conditions. The importance and the versatility of methods in the study of electrodes in contact with the electrolytes are described, when they are being cycled through the catalytic potentials during the progress of the oxygen-evolution, oxygen reduction and hydrogen evolution reactions. The catalytic oxygen evolution reaction is illustrated with examples using three oxides, Co, Ni and Mn, and two sulfides, Mo and Co. These are used as examples for the hydrogen evolution reaction. A bimetallic, bifunctional oxygen evolvingmore » and oxygen reducing Ni/Mn oxide is also presented. The various advantages and constraints in the use of these techniques and the future outlook are discussed.« less

Edge-illumination x-ray phase contrast imaging with Pt-based metallic glass masks

NASA Astrophysics Data System (ADS)

Saghamanesh, Somayeh; Aghamiri, Seyed Mahmoud-Reza; Olivo, Alessandro; Sadeghilarijani, Maryam; Kato, Hidemi; Kamali-Asl, Alireza; Yashiro, Wataru

2017-06-01

Edge-illumination x-ray phase contrast imaging (EI XPCI) is a non-interferometric phase-sensitive method where two absorption masks are employed. These masks are fabricated through a photolithography process followed by electroplating which is challenging in terms of yield as well as time- and cost-effectiveness. We report on the first implementation of EI XPCI with Pt-based metallic glass masks fabricated by an imprinting method. The new tested alloy exhibits good characteristics including high workability beside high x-ray attenuation. The fabrication process is easy and cheap, and can produce large-size masks for high x-ray energies within minutes. Imaging experiments show a good quality phase image, which confirms the potential of these masks to make the EI XPCI technique widely available and affordable.

A new on-axis micro-spectrophotometer for combining Raman, fluorescence and UV/Vis absorption spectroscopy with macromolecular crystallography at the Swiss Light Source

PubMed Central

Pompidor, Guillaume; Dworkowski, Florian S. N.; Thominet, Vincent; Schulze-Briese, Clemens; Fuchs, Martin R.

2013-01-01

The combination of X-ray diffraction experiments with optical methods such as Raman, UV/Vis absorption and fluorescence spectroscopy greatly enhances and complements the specificity of the obtained information. The upgraded version of the in situ on-axis micro-spectrophotometer, MS2, at the macromolecular crystallography beamline X10SA of the Swiss Light Source is presented. The instrument newly supports Raman and resonance Raman spectroscopy, in addition to the previously available UV/Vis absorption and fluorescence modes. With the recent upgrades of the spectral bandwidth, instrument stability, detection efficiency and control software, the application range of the instrument and its ease of operation were greatly improved. Its on-axis geometry with collinear X-ray and optical axes to ensure optimal control of the overlap of sample volumes probed by each technique is still unique amongst comparable facilities worldwide and the instrument has now been in general user operation for over two years. PMID:23955041

A new on-axis micro-spectrophotometer for combining Raman, fluorescence and UV/Vis absorption spectroscopy with macromolecular crystallography at the Swiss Light Source.

PubMed

Pompidor, Guillaume; Dworkowski, Florian S N; Thominet, Vincent; Schulze-Briese, Clemens; Fuchs, Martin R

2013-09-01

The combination of X-ray diffraction experiments with optical methods such as Raman, UV/Vis absorption and fluorescence spectroscopy greatly enhances and complements the specificity of the obtained information. The upgraded version of the in situ on-axis micro-spectrophotometer, MS2, at the macromolecular crystallography beamline X10SA of the Swiss Light Source is presented. The instrument newly supports Raman and resonance Raman spectroscopy, in addition to the previously available UV/Vis absorption and fluorescence modes. With the recent upgrades of the spectral bandwidth, instrument stability, detection efficiency and control software, the application range of the instrument and its ease of operation were greatly improved. Its on-axis geometry with collinear X-ray and optical axes to ensure optimal control of the overlap of sample volumes probed by each technique is still unique amongst comparable facilities worldwide and the instrument has now been in general user operation for over two years.

Accurate Modeling of X-ray Extinction by Interstellar Grains

NASA Astrophysics Data System (ADS)

Hoffman, John; Draine, B. T.

2016-02-01

Interstellar abundance determinations from fits to X-ray absorption edges often rely on the incorrect assumption that scattering is insignificant and can be ignored. We show instead that scattering contributes significantly to the attenuation of X-rays for realistic dust grain size distributions and substantially modifies the spectrum near absorption edges of elements present in grains. The dust attenuation modules used in major X-ray spectral fitting programs do not take this into account. We show that the consequences of neglecting scattering on the determination of interstellar elemental abundances are modest; however, scattering (along with uncertainties in the grain size distribution) must be taken into account when near-edge extinction fine structure is used to infer dust mineralogy. We advertise the benefits and accuracy of anomalous diffraction theory for both X-ray halo analysis and near edge absorption studies. We present an open source Fortran suite, General Geometry Anomalous Diffraction Theory (GGADT), that calculates X-ray absorption, scattering, and differential scattering cross sections for grains of arbitrary geometry and composition.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Di, Zichao; Chen, Si; Hong, Young Pyo

X-ray fluorescence tomography is based on the detection of fluorescence x-ray photons produced following x-ray absorption while a specimen is rotated; it provides information on the 3D distribution of selected elements within a sample. One limitation in the quality of sample recovery is the separation of elemental signals due to the finite energy resolution of the detector. Another limitation is the effect of self-absorption, which can lead to inaccurate results with dense samples. To recover a higher quality elemental map, we combine x-ray fluorescence detection with a second data modality: conventional x-ray transmission tomography using absorption. By using these combinedmore » signals in a nonlinear optimization-based approach, we demonstrate the benefit of our algorithm on real experimental data and obtain an improved quantitative reconstruction of the spatial distribution of dominant elements in the sample. Furthermore, compared with single-modality inversion based on x-ray fluorescence alone, this joint inversion approach reduces ill-posedness and should result in improved elemental quantification and better correction of self-absorption.« less

Electronic and atomic structures of Ti{sub 1-x}Al{sub x}N thin films related to their damage behavior

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tuilier, M.-H.; Pac, M.-J.; Girleanu, M.

2008-04-15

Ti and Al K-edge x-ray absorption spectroscopy is used to investigate the electronic structure of Ti{sub 1-x}Al{sub x}N thin films deposited by reactive magnetron sputtering. The experimental near edge spectra of TiN and AlN are interpreted in the light of unoccupied density of state band structure calculations. The comparison of the structural parameters derived from x-ray absorption fine structure and x-ray diffraction reveals segregation between Al-rich and Ti-rich domains within the Ti{sub 1-x}Al{sub x}N films. Whereas x-ray diffraction probes only the crystallized domains, the structural information derived from extended x-ray absorption fine structure analysis turns on both crystalline and grainmore » boundaries. The results are discussed by considering the damage behavior of the films depending on the composition.« less

Using measured 30-150 kVp polychromatic tungsten x-ray spectra to determine ion chamber calibration factors, Nx (Gy C(-1)).

PubMed

Mercier, J R; Kopp, D T; McDavid, W D; Dove, S B; Lancaster, J L; Tucker, D M

2000-10-01

Two methods for determining ion chamber calibration factors (Nx) are presented for polychromatic tungsten x-ray beams whose spectra differ from beams with known Nx. Both methods take advantage of known x-ray fluence and kerma spectral distributions. In the first method, the x-ray tube potential is unchanged and spectra of differing filtration are measured. A primary standard ion chamber with known Nx for one beam is used to calculate the x-ray fluence spectrum of a second beam. Accurate air energy absorption coefficients are applied to the x-ray fluence spectra of the second beam to calculate actual air kerma and Nx. In the second method, two beams of differing tube potential and filtration with known Nx are used to bracket a beam of unknown Nx. A heuristically derived Nx interpolation scheme based on spectral characteristics of all three beams is described. Both methods are validated. Both methods improve accuracy over the current half value layer Nx estimating technique.

Effect of Pressure on Valence and Structural Properties of YbFe 2 Ge 2 Heavy Fermion Compound—A Combined Inelastic X-ray Spectroscopy, X-ray Diffraction, and Theoretical Investigation

DOE PAGES

Kumar, Ravhi S.; Svane, Axel; Vaitheeswaran, Ganapathy; ...

2015-10-19

We measured the crystal structure and the Yb valence of the YbFe 2Ge 2 heavy fermion compound at room temperature and under high pressures using high-pressure powder X-ray diffraction and X-ray absorption spectroscopy via both partial fluorescence yield and resonant inelastic X-ray emission techniques. Moreover, the measurements are complemented by first-principles density functional theoretical calculations using the self-interaction corrected local spin density approximation investigating in particular the magnetic structure and the Yb valence. Finally, while the ThCr 2Si 2-type tetragonal (I4/mmm) structure is stable up to 53 GPa, the X-ray emission results show an increase of the Yb valence frommore » v = 2.72(2) at ambient pressure to v = 2.93(3) at ~9 GPa, where at low temperature a pressure-induced quantum critical state was reported.« less

ID16B: a hard X-ray nanoprobe beamline at the ESRF for nano-analysis

PubMed Central

Martínez-Criado, Gema; Villanova, Julie; Tucoulou, Rémi; Salomon, Damien; Suuronen, Jussi-Petteri; Labouré, Sylvain; Guilloud, Cyril; Valls, Valentin; Barrett, Raymond; Gagliardini, Eric; Dabin, Yves; Baker, Robert; Bohic, Sylvain; Cohen, Cédric; Morse, John

2016-01-01

Within the framework of the ESRF Phase I Upgrade Programme, a new state-of-the-art synchrotron beamline ID16B has been recently developed for hard X-ray nano-analysis. The construction of ID16B was driven by research areas with major scientific and societal impact such as nanotechnology, earth and environmental sciences, and bio-medical research. Based on a canted undulator source, this long beamline provides hard X-ray nanobeams optimized mainly for spectroscopic applications, including the combination of X-ray fluorescence, X-ray diffraction, X-ray excited optical luminescence, X-ray absorption spectroscopy and 2D/3D X-ray imaging techniques. Its end-station re-uses part of the apparatus of the earlier ID22 beamline, while improving and enlarging the spectroscopic capabilities: for example, the experimental arrangement offers improved lateral spatial resolution (∼50 nm), a larger and more flexible capability for in situ experiments, and monochromatic nanobeams tunable over a wider energy range which now includes the hard X-ray regime (5–70 keV). This paper describes the characteristics of this new facility, short-term technical developments and the first scientific results. PMID:26698084

Interatomic scattering in energy dependent photoelectron spectra of Ar clusters

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patanen, M.; Benkoula, S.; Nicolas, C.

2015-09-28

Soft X-ray photoelectron spectra of Ar 2p levels of atomic argon and argon clusters are recorded over an extended range of photon energies. The Ar 2p intensity ratios between atomic argon and clusters’ surface and bulk components reveal oscillations similar to photoelectron extended X-ray absorption fine structure signal (PEXAFS). We demonstrate here that this technique allows us to analyze separately the PEXAFS signals from surface and bulk sites of free-standing, neutral clusters, revealing a bond contraction at the surface.

One body, many heads; the Cerberus of catalysis. A new multipurpose in-situ cell for XAS at ALBA

NASA Astrophysics Data System (ADS)

Guilera, G.; Rey, F.; Hernández-Fenollosa, J.; Cortés-Vergaz, J. J.

2013-04-01

A new multi-purpose in-situ cell and its control system have been developed for synchrotron-based techniques as are X-Ray Absorption spectroscopy (XAS) and X-Ray Diffraction (XRD). The cell is made of a stainless steel 'body' and three different exchangeable 'heads' to tackle different scientific areas that include solid-gas catalysis, solid-liquid catalysis and electrocatalysis. The different versions of the cell are herein described and their functionality is exemplified by some case studies.

Resonant magnetic scattering of polarized soft x rays

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sacchi, M.; Hague, C.F.; Gullikson, E.M.

1997-04-01

Magnetic effects on X-ray scattering (Bragg diffraction, specular reflectivity or diffuse scattering) are a well known phenomenon, and they also represent a powerful tool for investigating magnetic materials since it was shown that they are strongly enhanced when the photon energy is tuned across an absorption edge (resonant process). The resonant enhancement of the magnetic scattering has mainly been investigated at high photon energies, in order to match the Bragg law for the typical lattice spacings of crystals. In the soft X-ray range, even larger effects are expected, working for instance at the 2p edges of transition metals of themore » first row or at the 3d edges of rare earths (300-1500 eV), but the corresponding long wavelengths prevent the use of single crystals. Two approaches have been recently adopted in this energy range: (i) the study of the Bragg diffraction from artificial structures of appropriate 2d spacing; (ii) the analysis of the specular reflectivity, which contains analogous information but has no constraints related to the lattice spacing. Both approaches have their own specific advantages: for instance, working under Bragg conditions provides information about the (magnetic) periodicity in ordered structures, while resonant reflectivity can easily be related to electronic properties and absorption spectra. An important aspect common to all the resonant X-ray scattering techniques is the element selectivity inherent to the fact of working at a specific absorption edge: under these conditions, X-ray scattering becomes in fact a spectroscopy. Results are presented for films of iron and cobalt.« less

Electronic structure measurements of metal-organic solar cell dyes using x-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Johnson, Phillip S.

The focus of this thesis is twofold: to report the results of X-ray absorption studies of metal-organic dye molecules for dye-sensitized solar cells and to provide a basic training manual on X-ray absorption spectroscopy techniques and data analysis. The purpose of our research on solar cell dyes is to work toward an understanding of the factors influencing the electronic structure of the dye: the choice of the metal, its oxidation state, ligands, and cage structure. First we study the effect of replacing Ru in several common dye structures by Fe. First-principles calculations and X-ray absorption spectroscopy at the C 1s and N 1s edges are combined to investigate transition metal dyes in octahedral and square planar N cages. Octahedral molecules are found to have a downward shift in the N 1s-to-pi* transition energy and an upward shift in C 1s-to-pi* transition energy when Ru is replaced by Fe, explained by an extra transfer of negative charge from Fe to the N ligands compared to Ru. For the square planar molecules, the behavior is more complex because of the influence of axial ligands and oxidation state. Next the crystal field parameters for a series of phthalocyanine and porphyrins dyes are systematically determined using density functional calculations and atomic multiplet calculations with polarization-dependent X-ray absorption spectra. The polarization dependence of the spectra provides information on orbital symmetries which ensures the determination of the crystal field parameters is unique. A uniform downward scaling of the calculated crystal field parameters by 5-30% is found to be necessary to best fit the spectra. This work is a part of the ongoing effort to design and test new solar cell dyes. Replacing the rare metal Ru with abundant metals like Fe would be a significant advance for dye-sensitized solar cells. Understanding the effects of changing the metal centers in these dyes in terms of optical absorption, charge transfer, and electronic structure enables the systematic design of new dyes using less expensive materials.

Growth and process identification of CuInS 2 on GaP by chemical vapor deposition

NASA Astrophysics Data System (ADS)

Hwang, H. L.; Sun, C. Y.; Fang, C. S.; Chang, S. D.; Cheng, C. H.; Yang, M. H.; Lin, H. H.; Tuwan-Mu, H.

1981-10-01

Experimental techniques for growing CuInS 2 layers on GaP substrates by the metalorganic method have been developed. Hydrogen sulfide gas together with the vapors of CuCl( NCCH3) n and InCl3( NCCH3) both of which were generated by bubbling nitrogen through sources, using a solvent of acetonitride, were used as transport agents. Various characterization techniques such as atomic absorption (AA), neutron activation analysis (NAA), energy dispersive analysis by X-rays (EDAX), Rutherford back-scattering analysis (RBS), and X-ray analyses were used to help understand the fundamental mechanism of the CVD growth.

Fast fluorescence techniques for crystallography beamlines

PubMed Central

Stepanov, Sergey; Hilgart, Mark; Yoder, Derek W.; Makarov, Oleg; Becker, Michael; Sanishvili, Ruslan; Ogata, Craig M.; Venugopalan, Nagarajan; Aragão, David; Caffrey, Martin; Smith, Janet L.; Fischetti, Robert F.

2011-01-01

This paper reports on several developments of X-ray fluorescence techniques for macromolecular crystallography recently implemented at the National Institute of General Medical Sciences and National Cancer Institute beamlines at the Advanced Photon Source. These include (i) three-band on-the-fly energy scanning around absorption edges with adaptive positioning of the fine-step band calculated from a coarse pass; (ii) on-the-fly X-ray fluorescence rastering over rectangular domains for locating small and invisible crystals with a shuttle-scanning option for increased speed; (iii) fluorescence rastering over user-specified multi-segmented polygons; and (iv) automatic signal optimization for reduced radiation damage of samples. PMID:21808424

Effect of X-ray irradiation on the optical absorption of СdSe1-xTex nanocrystals embedded in borosilicate glass

NASA Astrophysics Data System (ADS)

Prymak, M. V.; Azhniuk, Yu. M.; Solomon, A. M.; Krasilinets, V. M.; Lopushansky, V. V.; Bodnar, I. V.; Gomonnai, A. V.; Zahn, D. R. T.

2012-07-01

The effect of X-ray irradiation on the optical absorption spectra of CdSe1-xTex nanocrystals embedded in a borosilicate matrix is studied. The observed blue shift of the absorption edge and bleaching of the confinement-related features in the spectra are related to X-ray induced negative ionization of the nanocrystals with charge transfer across the nanocrystal/matrix interface. The radiation-induced changes are observed to recover after longer post-irradiation storage at room temperature.

Optical properties of Pr-doped BaY2F8

NASA Astrophysics Data System (ADS)

Andrade, Adriano B.; de Mello, Ana C. S.; Rezende, Marcos V. dos S.; Baldochi, Sonia L.; Valerio, Mário E. G.

2014-08-01

Crystalline samples of Pr-doped BaY2F8 (BaYF) were prepared by zone melting technique. The pure phase obtained was identified by X-ray diffraction measurement. Optical absorption result was evaluated and it showed that the formation of the absorption bands can be connected to color centers generated by radiation in the matrix. Radioluminescence emission measurements after excitation by X-ray showed that the material exhibited components responsible for long lasting phosphorescence. Short decay times were also evaluated, the measurements showed a fast component around 70 ns associated to the 4f15d1 → 4f2 transition of the Pr3+ ion. The Thermoluminescence (TL) results indicate the presence of two trapping centers.

Crystallography with online optical and X-ray absorption spectroscopies demonstrates an ordered mechanism in copper nitrite reductase.

PubMed

Hough, Michael A; Antonyuk, Svetlana V; Strange, Richard W; Eady, Robert R; Hasnain, S Samar

2008-04-25

Nitrite reductases are key enzymes that perform the first committed step in the denitrification process and reduce nitrite to nitric oxide. In copper nitrite reductases, an electron is delivered from the type 1 copper (T1Cu) centre to the type 2 copper (T2Cu) centre where catalysis occurs. Despite significant structural and mechanistic studies, it remains controversial whether the substrates, nitrite, electron and proton are utilised in an ordered or random manner. We have used crystallography, together with online X-ray absorption spectroscopy and optical spectroscopy, to show that X-rays rapidly and selectively photoreduce the T1Cu centre, but that the T2Cu centre does not photoreduce directly over a typical crystallographic data collection time. Furthermore, internal electron transfer between the T1Cu and T2Cu centres does not occur, and the T2Cu centre remains oxidised. These data unambiguously demonstrate an 'ordered' mechanism in which electron transfer is gated by binding of nitrite to the T2Cu. Furthermore, the use of online multiple spectroscopic techniques shows their value in assessing radiation-induced redox changes at different metal sites and demonstrates the importance of ensuring the correct status of redox centres in a crystal structure determination. Here, optical spectroscopy has shown a very high sensitivity for detecting the change in T1Cu redox state, while X-ray absorption spectroscopy has reported on the redox status of the T2Cu site, as this centre has no detectable optical absorption.

Automated generation and ensemble-learned matching of X-ray absorption spectra

NASA Astrophysics Data System (ADS)

Zheng, Chen; Mathew, Kiran; Chen, Chi; Chen, Yiming; Tang, Hanmei; Dozier, Alan; Kas, Joshua J.; Vila, Fernando D.; Rehr, John J.; Piper, Louis F. J.; Persson, Kristin A.; Ong, Shyue Ping

2018-12-01

X-ray absorption spectroscopy (XAS) is a widely used materials characterization technique to determine oxidation states, coordination environment, and other local atomic structure information. Analysis of XAS relies on comparison of measured spectra to reliable reference spectra. However, existing databases of XAS spectra are highly limited both in terms of the number of reference spectra available as well as the breadth of chemistry coverage. In this work, we report the development of XASdb, a large database of computed reference XAS, and an Ensemble-Learned Spectra IdEntification (ELSIE) algorithm for the matching of spectra. XASdb currently hosts more than 800,000 K-edge X-ray absorption near-edge spectra (XANES) for over 40,000 materials from the open-science Materials Project database. We discuss a high-throughput automation framework for FEFF calculations, built on robust, rigorously benchmarked parameters. FEFF is a computer program uses a real-space Green's function approach to calculate X-ray absorption spectra. We will demonstrate that the ELSIE algorithm, which combines 33 weak "learners" comprising a set of preprocessing steps and a similarity metric, can achieve up to 84.2% accuracy in identifying the correct oxidation state and coordination environment of a test set of 19 K-edge XANES spectra encompassing a diverse range of chemistries and crystal structures. The XASdb with the ELSIE algorithm has been integrated into a web application in the Materials Project, providing an important new public resource for the analysis of XAS to all materials researchers. Finally, the ELSIE algorithm itself has been made available as part of veidt, an open source machine-learning library for materials science.

Discovery of an X-ray Violently Variable Broad Absorption Line Quasar

NASA Technical Reports Server (NTRS)

Ghosh, Kajal K.; Gutierrez, Carlos M.; Punsly, Brian; Chevallier, Loic; Goncalves, Anabela C.

2006-01-01

In this letter, we report on a quasar that is violently variable in the X-rays, XVV. It is also a broad absorption line quasar (BALQSO) that exhibits both high ionization and low ionization UV absorption lines (LoBALQSO). It is very luminous in the X-rays (approximately 10(exp 46) ergs s(sup -l) over the entire X-ray band). Surprisingly, this does not over ionize the LoBAL outflow. The X-rays vary by a factor of two within minutes in the quasar rest frame, which is shorter than 1/30 of the light travel time across a scale length equal to the black hole radius. We concluded that the X-rays are produced in a relativistic jet beamed toward earth in which variations in the Doppler enhancement produce the XVV behavior.

Investigation and Control of "Sphere-Like" Buckminsterfullerene C60 and "Disk-Like" Copper(II) Phthalocyanine

NASA Astrophysics Data System (ADS)

McAfee, Terry Richard

Due to the growing global need for cheap, flexible, and portable electronics, numerous research groups from mechanical and electrical engineering, material science, chemistry, and physics have increasingly turned to organic electronics research over the last ˜5--10 years. Largely, the focus of researchers in this growing field have sought to obtain the next record holding device, allowing a heuristic approach of trial and error to become dominant focus of research rather than a fundamental understanding. Rather than working with the latest high performance organic semiconducting materials and film processing techniques, I have chosen to investigate and control the fundamental self-assembly interactions of organic photovoltaic thin films using simplified systems. Specifically, I focus on organic photovoltaic research using two of the oldest and well studies semiconducting materials, namely "sphere-like" electron donor material Buckminsterfullerene C60 and "disklike" electron acceptor material Copper(II) Phthalocyanine. I manufactured samples using the well-known technique of physical vapor deposition using a high vacuum chamber that I designed and built to accommodate my need of precise material deposition control, with codeposition capability. Films were characterized using microscopy and spectroscopy techniques locally at NCSU, including Atomic Force Microscopy, scanning tunneling microscopy, X-ray photoelectron spectroscopy, and Ultraviolet-visible spectroscopy, as well as at National Laboratory based synchrotron x-ray techniques, including Carbon and Nitrogen k-edge Total Electron Yield and Transmission Near Edge X-ray absorption fine structure spectroscopy, Carbon k-edge Resonant Soft x-ray Microscopy, Resonant Soft x-ray reflectivity, and Grazing Incidence Wide-Angle X-ray scattering.

A Highly Sensitive X-ray Imaging Modality for Hepatocellular Carcinoma Detection in Vitro

PubMed Central

Rand, Danielle; Walsh, Edward G.; Derdak, Zoltan; Wands, Jack R.; Rose-Petruck, Christoph

2015-01-01

Innovations that improve sensitivity and reduce cost are of paramount importance in diagnostic imaging. The novel x-ray imaging modality called Spatial Frequency Heterodyne Imaging (SFHI) is based on a linear arrangement of x-ray source, tissue, and x-ray detector, much like that of a conventional x-ray imaging apparatus. However, SFHI rests on a complete paradigm reversal compared to conventional x-ray absorption-based radiology: while scattered x-rays are carefully rejected in absorption-based x-ray radiology to enhance the image contrast, SFHI forms images exclusively from x-rays scattered by the tissue. In this study we use numerical processing to produce x-ray scatter images of Hepatocellular Carcinoma (HCC) labeled with a nanoparticle contrast agent. We subsequently compare the sensitivity of SFHI in this application to that of both conventional x-ray imaging and Magnetic Resonance Imaging (MRI). Although SFHI is still in the early stages of its development, our results show that the sensitivity of SFHI is an order of magnitude greater than that of absorption-based x-ray imaging and approximately equal to that of MRI. As x-ray imaging modalities typically have lower installation and service costs compared to MRI, SFHI could become a cost effective alternative to MRI, particularly in areas of the world with inadequate availability of MRI facilities. PMID:25559398

A highly sensitive x-ray imaging modality for hepatocellular carcinoma detection in vitro

DOE PAGES

Rand, Danielle; Walsh, Edward G.; Derdak, Zoltan; ...

2015-01-05

Innovations that improve sensitivity and reduce cost are of paramount importance in diagnostic imaging. The novel x-ray imaging modality called Spatial Frequency Heterodyne Imaging (SFHI) is based on a linear arrangement of x-ray source, tissue, and x-ray detector, much like that of a conventional x-ray imaging apparatus. However, SFHI rests on a complete paradigm reversal compared to conventional x-ray absorption-based radiology: while scattered x-rays are carefully rejected in absorption-based x-ray radiology to enhance the image contrast, SFHI forms images exclusively from x-rays scattered by the tissue. Here in this study we use numerical processing to produce x-ray scatter images ofmore » Hepatocellular Carcinoma (HCC) labeled with a nanoparticle contrast agent. We subsequently compare the sensitivity of SFHI in this application to that of both conventional x-ray imaging and Magnetic Resonance Imaging (MRI). Although SFHI is still in the early stages of its development, our results show that the sensitivity of SFHI is an order of magnitude greater than that of absorption-based x-ray imaging and approximately equal to that of MRI. Lastly, as x-ray imaging modalities typically have lower installation and service costs compared to MRI, SFHI could become a cost effective alternative to MRI, particularly in areas of the world with inadequate availability of MRI facilities.« less

Local Structure Determination of Carbon/Nickel Ferrite Composite Nanofibers Probed by X-ray Absorption Spectroscopy.

PubMed

Nilmoung, Sukunya; Kidkhunthod, Pinit; Maensiri, Santi

2015-11-01

Carbon/NiFe2O4 composite nanofibers have been successfully prepared by electrospinning method using a various concentration solution of Ni and Fe nitrates dispersed into polyacrylonitride (PAN) solution in N,N' dimethylformamide. The phase and mophology of PAN/NiFe2O4 composite samples were characterized and investigated by X-ray diffraction and scanning electron microscopy. The magnetic properties of the prepared samples were measured at ambient temperature by a vibrating sample magnetometer. It is found that all composite samples exhibit ferromagnetism. This could be local-structurally explained by the existed oxidation states of Ni2+ and Fe3+ in the samples. Moreover, local environments around Ni and Fe ions could be revealed by X-ray absorption spectroscopy (XAS) measurement including X-ray absorption near edge structure (XANES) and Extended X-ray absorption fine structure (EXAFS).

Detection of absorption lines in the spectra of X-ray bursts from X1608-52

NASA Astrophysics Data System (ADS)

Nakamura, Norio; Inoue, Hajime; Tanaka, Yasuo

X-ray bursts from X 1608-52 were observed with the gas scintillation proportional counters on the Tenma satellite. Absorption features were detected in the spectra of three bursts among 17 bursts observed. These absorption features are consistent with a common absorption line at 4.1 keV. The energy and the properties of the absorption lines of the X 1608-52 bursts are very similar to those observed from the X 1636-53 bursts by Waki et al. (1984). Near equality of the absorption-line energies for X 1636-53 and X 1608-52 would imply that mass and radius of the neutron stars in these two systems are very similar to each other.

Resonant inelastic X-ray scattering on synthetic nickel compounds and Ni-Fe hydrogenase protein

NASA Astrophysics Data System (ADS)

Sanganas, Oliver; Löscher, Simone; Pfirrmann, Stefan; Marinos, Nicolas; Glatzel, Pieter; Weng, Tsu-Chien; Limberg, Christian; Driess, Matthias; Dau, Holger; Haumann, Michael

2009-11-01

Ni-Fe hydrogenases are proteins catalyzing the oxidative cleavage of dihydrogen (H2) and proton reduction to H2 at high turnover rates. Their active site is a heterobimetallic center comprising one Ni and one Fe atom. To understand the function of the site, well resolved structural and electronic information is required. Such information is expected to become accessible by high resolution X-ray absorption and emission techniques, which are rapidly developing at third generation synchrotron radiation sources. We studied a number of synthetic Ni compounds, which mimic relevant features of the Ni site in hydrogenases, and the Ni site in the soluble, NAD-reducing hydrogenase (SH) from the bacterium Ralstonia eutropha by resonant inelastic X-ray scattering (RIXS) using a Rowland-type spectrometer at the ESRF. The SH is particularly interesting because its H2-cleavage reaction is highly resistant against inhibition by O2. Kα-fluorescence detected RIXS planes in the 1s→3d region of the X-ray absorption spectrum were recorded on the protein which allow to extract L3-edge type spectra Spectral features of the protein are compared to those of the model compounds.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Lidong; Zhou, Lu; Ould-Chikh, Samy

Surface composition and structure are of vital importance for heterogeneous catalysts, especially for bimetallic catalysts, which often vary as a function of reaction conditions (known as surface segregation). The preparation of bimetallic catalysts with controlled metal surface composition and structure is very challenging. In this study, we synthesize a series of Ni/Pt bimetallic catalysts with controlled metal surface composition and structure using a method derived from surface organometallic chemistry. The evolution of the surface composition and structure of the obtained bimetallic catalysts under simulated reaction conditions is investigated by various techniques, which include CO-probe IR spectroscopy, high-angle annular dark-field scanningmore » transmission electron microscopy, energy-dispersive X-ray spectroscopy, extended X-ray absorption fine structure analysis, X-ray absorption near-edge structure analysis, XRD, and X-ray photoelectron spectroscopy. It is demonstrated that the structure of the bimetallic catalyst is evolved from Pt monolayer island-modified Ni nanoparticles to core–shell bimetallic nanoparticles composed of a Ni-rich core and a Ni/Pt alloy shell upon thermal treatment. As a result, these catalysts are active for the dry reforming of methane, and their catalytic activities, stabilities, and carbon formation vary with their surface composition and structure.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Lidong; Zhou, Lu; Ould-Chikh, Samy

The surface composition and structure are of vital importance for heterogeneous catalysts, especially for bimetallic catalysts, which often vary as a function of reaction conditions (known as surface segregation). The preparation of bimetallic catalysts with controlled metal surface composition and structure is very challenging. In this study, we synthesize a series of Ni/Pt bimetallic catalysts with controlled metal surface composition and structure using a method derived from surface organometallic chemistry. Moreover, the evolution of the surface composition and structure of the obtained bimetallic catalysts under simulated reaction conditions is investigated by various techniques, which include CO-probe IR spectroscopy, high-angle annularmore » dark-field scanning transmission electron microscopy, energy-dispersive X-ray spectroscopy, extended X-ray absorption fine structure analysis, X-ray absorption near-edge structure analysis, XRD, and X-ray photoelectron spectroscopy. It is demonstrated that the structure of the bimetallic catalyst is evolved from Pt monolayer island-modified Ni nanoparticles to core–shell bimetallic nanoparticles composed of a Ni-rich core and a Ni/Pt alloy shell upon thermal treatment. The catalysts are active for the dry reforming of methane, and their catalytic activities, stabilities, and carbon formation vary with their surface composition and structure.« less

Development of picosecond time-resolved X-ray absorption spectroscopy by high-repetition-rate laser pump/X-ray probe at Beijing Synchrotron Radiation Facility.

PubMed

Wang, Hao; Yu, Can; Wei, Xu; Gao, Zhenhua; Xu, Guang Lei; Sun, Da Rui; Li, Zhenjie; Zhou, Yangfan; Li, Qiu Ju; Zhang, Bing Bing; Xu, Jin Qiang; Wang, Lin; Zhang, Yan; Tan, Ying Lei; Tao, Ye

2017-05-01

A new setup and commissioning of transient X-ray absorption spectroscopy are described, based on the high-repetition-rate laser pump/X-ray probe method, at the 1W2B wiggler beamline at the Beijing Synchrotron Radiation Facility. A high-repetition-rate and high-power laser is incorporated into the setup with in-house-built avalanche photodiodes as detectors. A simple acquisition scheme was applied to obtain laser-on and laser-off signals simultaneously. The capability of picosecond transient X-ray absorption spectroscopy measurement was demonstrated for a photo-induced spin-crossover iron complex in 6 mM solution with 155 kHz repetition rate.

Factors influencing real time internal structural visualization and dynamic process monitoring in plants using synchrotron-based phase contrast X-ray imaging

PubMed Central

Karunakaran, Chithra; Lahlali, Rachid; Zhu, Ning; Webb, Adam M.; Schmidt, Marina; Fransishyn, Kyle; Belev, George; Wysokinski, Tomasz; Olson, Jeremy; Cooper, David M. L.; Hallin, Emil

2015-01-01

Minimally invasive investigation of plant parts (root, stem, leaves, and flower) has good potential to elucidate the dynamics of plant growth, morphology, physiology, and root-rhizosphere interactions. Laboratory based absorption X-ray imaging and computed tomography (CT) systems are extensively used for in situ feasibility studies of plants grown in natural and artificial soil. These techniques have challenges such as low contrast between soil pore space and roots, long X-ray imaging time, and low spatial resolution. In this study, the use of synchrotron (SR) based phase contrast X-ray imaging (PCI) has been demonstrated as a minimally invasive technique for imaging plants. Above ground plant parts and roots of 10 day old canola and wheat seedlings grown in sandy clay loam soil were successfully scanned and reconstructed. Results confirmed that SR-PCI can deliver good quality images to study dynamic and real time processes such as cavitation and water-refilling in plants. The advantages of SR-PCI, effect of X-ray energy, and effective pixel size to study plant samples have been demonstrated. The use of contrast agents to monitor physiological processes in plants was also investigated and discussed. PMID:26183486

Large field of view, fast and low dose multimodal phase-contrast imaging at high x-ray energy.

PubMed

Astolfo, Alberto; Endrizzi, Marco; Vittoria, Fabio A; Diemoz, Paul C; Price, Benjamin; Haig, Ian; Olivo, Alessandro

2017-05-19

X-ray phase contrast imaging (XPCI) is an innovative imaging technique which extends the contrast capabilities of 'conventional' absorption based x-ray systems. However, so far all XPCI implementations have suffered from one or more of the following limitations: low x-ray energies, small field of view (FOV) and long acquisition times. Those limitations relegated XPCI to a 'research-only' technique with an uncertain future in terms of large scale, high impact applications. We recently succeeded in designing, realizing and testing an XPCI system, which achieves significant steps toward simultaneously overcoming these limitations. Our system combines, for the first time, large FOV, high energy and fast scanning. Importantly, it is capable of providing high image quality at low x-ray doses, compatible with or even below those currently used in medical imaging. This extends the use of XPCI to areas which were unpractical or even inaccessible to previous XPCI solutions. We expect this will enable a long overdue translation into application fields such as security screening, industrial inspections and large FOV medical radiography - all with the inherent advantages of the XPCI multimodality.

Measuring partial fluorescence yield using filtered detectors.

PubMed

Boyko, T D; Green, R J; Moewes, A; Regier, T Z

2014-07-01

Typically, X-ray absorption near-edge structure measurements aim to probe the linear attenuation coefficient. These measurements are often carried out using partial fluorescence yield techniques that rely on detectors having photon energy discrimination improving the sensitivity and the signal-to-background ratio of the measured spectra. However, measuring the partial fluorescence yield in the soft X-ray regime with reasonable efficiency requires solid-state detectors, which have limitations due to the inherent dead-time while measuring. Alternatively, many of the available detectors that are not energy dispersive do not suffer from photon count rate limitations. A filter placed in front of one of these detectors will make the energy-dependent efficiency non-linear, thereby changing the responsivity of the detector. It is shown that using an array of filtered X-ray detectors is a viable method for measuring soft X-ray partial fluorescence yield spectra without dead-time. The feasibility of this technique is further demonstrated using α-Fe2O3 as an example and it is shown that this detector technology could vastly improve the photon collection efficiency at synchrotrons and that these detectors will allow experiments to be completed with a much lower photon flux reducing X-ray-induced damage.

Preliminary in situ and real-time study of directional solidification of metallic alloys by x-ray imaging techniques

NASA Astrophysics Data System (ADS)

Nguyen Thi, H.; Jamgotchian, H.; Gastaldi, J.; Härtwig, J.; Schenk, T.; Klein, H.; Billia, B.; Baruchel, J.; Dabo, Y.

2003-05-01

During directional solidification of a binary alloy, the solid-liquid interface exhibits a variety of patterns that are due to the Mullins-Sekerka instability and governed by the growth conditions. It is well known that properties of the grown material are largely controlled by the microstructures left in the solid during processing. Thus, a precise mastering of the solidification is essential to tailor products in a reproducible fashion to a specified quality. One major difficulty for this study is the real-time and in situ observation of the interface, especially for metallic alloys. A possibility is to use an intense and coherent third generation x-ray beam. By combining different x-ray imaging techniques (absorption/phase contrast radiography and diffraction topography), we have studied the directional melting and solidification of aluminium-based alloys. The preliminary results show the great potential of these techniques for the study of the coupling between stress effects and microstructure formation in solidification processing.

Selenium Metabolism in Cancer Cells: The Combined Application of XAS and XFM Techniques to the Problem of Selenium Speciation in Biological Systems

PubMed Central

Weekley, Claire M.; Aitken, Jade B.; Finney, Lydia; Vogt, Stefan; Witting, Paul K.; Harris, Hugh H.

2013-01-01

Determining the speciation of selenium in vivo is crucial to understanding the biological activity of this essential element, which is a popular dietary supplement due to its anti-cancer properties. Hyphenated techniques that combine separation and detection methods are traditionally and effectively used in selenium speciation analysis, but require extensive sample preparation that may affect speciation. Synchrotron-based X-ray absorption and fluorescence techniques offer an alternative approach to selenium speciation analysis that requires minimal sample preparation. We present a brief summary of some key HPLC-ICP-MS and ESI-MS/MS studies of the speciation of selenium in cells and rat tissues. We review the results of a top-down approach to selenium speciation in human lung cancer cells that aims to link the speciation and distribution of selenium to its biological activity using a combination of X-ray absorption spectroscopy (XAS) and X-ray fluorescence microscopy (XFM). The results of this approach highlight the distinct fates of selenomethionine, methylselenocysteine and selenite in terms of their speciation and distribution within cells: organic selenium metabolites were widely distributed throughout the cells, whereas inorganic selenium metabolites were compartmentalized and associated with copper. New data from the XFM mapping of electrophoretically-separated cell lysates show the distribution of selenium in the proteins of selenomethionine-treated cells. Future applications of this top-down approach are discussed. PMID:23698165

Effect of Fe-substitution on the structure and magnetism of single crystals Mn2-xFexBO4

NASA Astrophysics Data System (ADS)

Platunov, M. S.; Kazak, N. V.; Knyazev, Yu. V.; Bezmaternykh, L. N.; Moshkina, E. M.; Trigub, A. L.; Veligzhanin, A. A.; Zubavichus, Y. V.; Solovyov, L. A.; Velikanov, D. A.; Ovchinnikov, S. G.

2017-10-01

Single crystalline Mn2-xFexBO4 with x = 0.3, 0.5, 0.7 grown by the flux method have been studied by means of X-ray diffraction and X-ray absorption spectroscopy at both Mn and Fe K edges. The compounds were found to crystallize in an orthorhombic warwickite structure (sp. gr. Pnam). The lattice parameters change linearly with x thus obeying the Vegard's law. The Fe3+ substitution for Mn3+ has been deduced from the X-ray absorption near-edge structure (XANES) spectra. Two energy positions of the absorption edges have been observed in Mn K-edge XANES spectra indicating the presence of manganese in two different oxidation states. Extended X-ray absorption fine structure (EXAFS) analysis has shown the reduction of local structural distortions upon Fe substitution. The magnetization data have revealed a spin-glass transition at TSG = 11, 14 and 18 K for x = 0.3, 0.5 and 0.7, respectively.

Topographic measurement of buried thin-film interfaces using a grazing resonant soft x-ray scattering technique

NASA Astrophysics Data System (ADS)

Gann, Eliot; Watson, Anne; Tumbleston, John R.; Cochran, Justin; Yan, Hongping; Wang, Cheng; Seok, Jaewook; Chabinyc, Michael; Ade, Harald

2014-12-01

The internal structures of thin films, particularly interfaces between different materials, are critical to system properties and performance across many disciplines, but characterization of buried interface topography is often unfeasible. In this work, we demonstrate that grazing resonant soft x-ray scattering (GRSoXS), a technique measuring diffusely scattered soft x rays from grazing incidence, can reveal the statistical topography of buried thin-film interfaces. By controlling and predicting the x-ray electric field intensity throughout the depth of the film and simultaneously the scattering contrast between materials, we are able to unambiguously identify the microstructure at different interfaces of a model polymer bilayer system. We additionally demonstrate the use of GRSoXS to selectively measure the topography of the surface and buried polymer-polymer interface in an organic thin-film transistor, revealing different microstructure and markedly differing evolution upon annealing. In such systems, where only indirect control of interface topography is possible, accurate measurement of the structure of interfaces for feedback is critically important. While we demonstrate the method here using organic materials, we also show that the technique is readily extendable to any thin-film system with elemental or chemical contrasts exploitable at absorption edges.

EUV Spectroscopy of High-redshift X-ray Objects

NASA Astrophysics Data System (ADS)

Kowalski, Michael Paul; Wolff, M. T.; Wood, K. S.; Barbee, T. W., Jr.

2010-03-01

As astronomical observations are pushed to cosmological distances (z>3) the spectral energy distributions of X-ray objects, AGNs for example, will have their maxima redshifted into the EUV waveband ( 90-912 Å/0.1-0.01 keV). Consequently, a wealth of spectral diagnostics, provided by, for example, the Fe L-shell complex ( 60-6 Å/0.2-2.0 keV) and the O VII/VIII lines ( 20 Å/0.5 keV), will be lost to X-ray instruments operating at traditional ( 0.5-10 keV) and higher X-ray energies. There are precedents in other wavebands. For example, HST evolutionary studies will become largely the province of JWST. Despite the successes of EUVE, the ROSAT WFC, and the Chandra LETG, the EUV continues to be unappreciated and under-utilized, partly because of a preconception that absorption by neutral galactic Hydrogen in the ISM prevents any useful extragalactic measurements at all EUV wavelengths and, until recently, by a lack of a suitable enabling technology. Thus, if future planned X-ray missions (e.g., IXO, Gen-X) are optimized again for traditional X-ray energies, their performance (effective area, resolving power) will be cut off at ultrasoft X-ray energies or at best be radically reduced in the EUV. This opens up a critical gap in performance located right at short EUV wavelengths, where the critical X-ray spectral transitions occur in high-z objects. However, normal-incidence multilayer-grating technology, which performs best precisely at such wavelengths, together with advanced nano-laminate fabrication techniques have been developed and are now mature to the point where advanced EUV instrument designs with performance complementary to IXO and Gen-X are practical. Such EUV instruments could be flown either independently or as secondary instruments on these X-ray missions. We present here a critical examination of the limits placed on extragalactic EUV measurements by ISM absorption, the range where high-z measurements are practical, and the requirements this imposes on next-generation instrument designs.

Composition Analysis of III-Nitrides at the Nanometer Scale: Comparison of Energy Dispersive X-ray Spectroscopy and Atom Probe Tomography.

PubMed

Bonef, Bastien; Lopez-Haro, Miguel; Amichi, Lynda; Beeler, Mark; Grenier, Adeline; Robin, Eric; Jouneau, Pierre-Henri; Mollard, Nicolas; Mouton, Isabelle; Monroy, Eva; Bougerol, Catherine

2016-12-01

The enhancement of the performance of advanced nitride-based optoelectronic devices requires the fine tuning of their composition, which has to be determined with a high accuracy and at the nanometer scale. For that purpose, we have evaluated and compared energy dispersive X-ray spectroscopy (EDX) in a scanning transmission electron microscope (STEM) and atom probe tomography (APT) in terms of composition analysis of AlGaN/GaN multilayers. Both techniques give comparable results with a composition accuracy better than 0.6 % even for layers as thin as 3 nm. In case of EDX, we show the relevance of correcting the X-ray absorption by simultaneous determination of the mass thickness and chemical composition at each point of the analysis. Limitations of both techniques are discussed when applied to specimens with different geometries or compositions.

Bandpass x-ray diode and x-ray multiplier detector

DOEpatents

Wang, C.L.

1982-09-27

An absorption-edge of an x-ray absorption filter and a quantum jump of a photocathode determine the bandpass characteristics of an x-ray diode detector. An anode, which collects the photoelectrons emitted by the photocathode, has enhanced amplification provided by photoelectron-multiplying means which include dynodes or a microchannel-plate electron-multiplier. Suppression of undesired high frequency response for a bandpass x-ray diode is provided by subtracting a signal representative of energies above the passband from a signal representative of the overall response of the bandpass diode.

Synchrotron X-ray microfluorescence measurement of metal distributions in Phragmites australis root system in the Yangtze River intertidal zone

DOE Office of Scientific and Technical Information (OSTI.GOV)

Feng, Huan; Zhang, Weiguo; Qian, Yu

2016-06-15

This study investigates the distributions of Br, Ca, Cl, Cr, Cu, K, Fe, Mn, Pb, Ti, V and Zn inPhragmites australisroot system and the function of Fe nanoparticles in scavenging metals in the root epidermis using synchrotron X-ray microfluorescence, synchrotron transmission X-ray microscope measurement and synchrotron X-ray absorption near-edge structure techniques. The purpose of this study is to understand the mobility of metals in wetland plant root systems after their uptake from rhizosphere soils.Phragmites australissamples were collected in the Yangtze River intertidal zone in July 2013. The results indicate that Fe nanoparticles are present in the root epidermis and thatmore » other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis.« less

Scanning Transmission X-ray Microscopy: Applications in Atmospheric Aerosol Research

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moffet, Ryan C.; Tivanski, Alexei V.; Gilles, Mary K.

Scanning transmission x-ray microscopy (STXM) combines x-ray microscopy and near edge x-ray absorption fine structure spectroscopy (NEXAFS). This combination provides spatially resolved bonding and oxidation state information. While there are reviews relevant to STXM/NEXAFS applications in other environmental fields (and magnetic materials) this chapter focuses on atmospheric aerosols. It provides an introduction to this technique in a manner approachable to non-experts. It begins with relevant background information on synchrotron radiation sources and a description of NEXAFS spectroscopy. The bulk of the chapter provides a survey of STXM/NEXAFS aerosol studies and is organized according to the type of aerosol investigated. Themore » purpose is to illustrate the current range and recent growth of scientific investigations employing STXM-NEXAFS to probe atmospheric aerosol morphology, surface coatings, mixing states, and atmospheric processing.« less

ACCURATE MODELING OF X-RAY EXTINCTION BY INTERSTELLAR GRAINS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoffman, John; Draine, B. T., E-mail: jah5@astro.princeton.edu, E-mail: draine@astro.princeton.edu

Interstellar abundance determinations from fits to X-ray absorption edges often rely on the incorrect assumption that scattering is insignificant and can be ignored. We show instead that scattering contributes significantly to the attenuation of X-rays for realistic dust grain size distributions and substantially modifies the spectrum near absorption edges of elements present in grains. The dust attenuation modules used in major X-ray spectral fitting programs do not take this into account. We show that the consequences of neglecting scattering on the determination of interstellar elemental abundances are modest; however, scattering (along with uncertainties in the grain size distribution) must bemore » taken into account when near-edge extinction fine structure is used to infer dust mineralogy. We advertise the benefits and accuracy of anomalous diffraction theory for both X-ray halo analysis and near edge absorption studies. We present an open source Fortran suite, General Geometry Anomalous Diffraction Theory (GGADT), that calculates X-ray absorption, scattering, and differential scattering cross sections for grains of arbitrary geometry and composition.« less

The Nature of the UV/X-ray Absorber In PG 2302+029

NASA Technical Reports Server (NTRS)

Sabra, Bassem M.; Hamann, Fred; Jannuzi, Buell T.; George, Ian M.; Shields, Joseph C.

2003-01-01

We present Chandra X-ray observations of the radio-quiet QSO PG 2302+029. This quasar has a rare system of ultra-high velocity (-56,000 km s(exp -1) UV absorption lines that form in an outflow from the active nucleus. The Chandra data indicate that soft X-ray absorption is also present. We perform a joint UV and X-ray analysis, using photoionization calculations, to determine the nature of the absorbing gas. The UV and X-ray datasets were not obtained simultaneously. Nonetheless, our analysis suggests that the X-ray absorption occurs at high velocities in the same general region as the UV absorber. There are not enough constraints to rule out multi-zone models. In fact, the distinct broad and narrow UV line profiles clearly indicate that multiple zones are present. Our preferred estimates of the ionization and total column density in the X-ray absorber (logU = 1.6, N(sub eta) = 10(exp 22.4) cm (exp -2) over predict the O VI lambda lambda1032,1038 absorption unless the X-ray absorber is also outflowing at approximately 56,000 km s(exp-l), but they over predict the Ne VIII lambda lambda 770,780 absorption at all velocities. If we assume that the X-ray absorbing gas is outflowing at the same velocity of the UV-absorbing wind and that the wind is radiatively accelerated, then the outflow must be launched at a radius of less than or equal to 10(exp 15) cm from the central continuum source. The smallness of this radius casts doubts on the assumption of radiative acceleration.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Jeongho; Kim, Kyung Hwan; Oang, Key Young

Characterization of transient molecular structures formed during chemical and biological processes is essential for understanding their mechanisms and functions. Over the last decade, time-resolved X-ray liquidography (TRXL) and time-resolved X-ray absorption spectroscopy (TRXAS) have emerged as powerful techniques for molecular and electronic structural analysis of photoinduced reactions in the solution phase. Both techniques make use of a pump–probe scheme that consists of (1) an optical pump pulse to initiate a photoinduced process and (2) an X-ray probe pulse to monitor changes in the molecular structure as a function of time delay between pump and probe pulses. TRXL is sensitive tomore » changes in the global molecular structure and therefore can be used to elucidate structural changes of reacting solute molecules as well as the collective response of solvent molecules. On the other hand, TRXAS can be used to probe changes in both local geometrical and electronic structures of specific X-ray-absorbing atoms due to the element-specific nature of core-level transitions. These techniques are complementary to each other and a combination of the two methods will enhance the capability of accurately obtaining structural changes induced by photoexcitation. Here we review the principles of TRXL and TRXAS and present recent application examples of the two methods for studying chemical and biological processes in solution. Furthermore, we briefly discuss the prospect of using X-ray free electron lasers for the two techniques, which will allow us to keep track of structural dynamics on femtosecond time scales in various solution-phase molecular reactions.« less

Atomic origin of the spin-polarization of the Co2FeAl Heusler compound

NASA Astrophysics Data System (ADS)

Liang, Jaw-Yeu; Lam, Tu-Ngoc; Lin, Yan-Cheng; Chang, Shu-Jui; Lin, Hong-Ji; Tseng, Yuan-Chieh

2016-02-01

Using synchrotron x-ray techniques, we studied the Co2FeAl spin-polarization state that generates the half-metallicity of the compound during an A2 (low-spin)  →  B2 (high-spin) phase transition. Given the advantage of element specificity of x-ray techniques, we could fingerprint the structural and magnetic cross-reactions between Co and Fe within a complex Co2FeAl structure deposited on a MgO (0 0 1) substrate. X-ray diffraction and extended x-ray absorption fine structure investigations determined that the Co atoms preferably populate the (1/4,1/4,1/4) and (3/4,3/4,3/4) sites during the development of the B2 phase. X-ray magnetic spectroscopy showed that although the two magnetic elements were ferromagnetically coupled, they interacted in a competing manner via a charge-transfer effect, which enhanced Co spin polarization at the expense of Fe spin polarization during the phase transition. This means that the spin-polarization of Co2FeAl was electronically dominated by Fe in A2 whereas the charge transfer turned the dominance to Co upon B2 formation. Helicity-dependent x-ray absorption spectra also revealed that only the minority state of Co/Fe was involved in the charge-transfer effect whereas the majority state was independent of it. Despite an overall increase of Co2FeAl magnetization, the charge-transfer effect created an undesired trade-off during the Co-Fe exchange interactions, because of the presence of twice as many X sites (Co) as Y sites (Fe) in the Heusler X 2 YZ formula. This suggests that the spin-polarization of Co2FeAl is unfortunately regulated by compromising the enhanced X (Co) sites and the suppressed Y (Fe) sites, irrespective of the development of the previously known high-spin-polarization phase of B2. This finding provides a possible cause for the limited half-metallicity of Co2FeAl discovered recently. Electronic tuning between the X and Y sites is necessary to further increase the spin-polarization, and likely the half-metallicity as well, of the compound.

X-ray absorption fine structure and x-ray diffraction studies of crystallographic grains in nanocrystalline FePd:Cu thin films

NASA Astrophysics Data System (ADS)

Krupinski, M.; Perzanowski, M.; Polit, A.; Zabila, Y.; Zarzycki, A.; Dobrowolska, A.; Marszalek, M.

2011-03-01

FePd alloys have recently attracted considerable attention as candidates for ultrahigh density magnetic storage media. In this paper we investigate FePd thin alloy film with a copper admixture composed of nanometer-sized grains. [Fe(0.9 nm)/Pd(1.1 nm)/Cu(d nm)]×5 multilayers were prepared by thermal deposition at room temperature in UHV conditions on Si(100) substrates covered by 100 nm SiO2. The thickness of the copper layer has been changed from 0 to 0.4 nm. After deposition, the multilayers were rapidly annealed at 600 °C in a nitrogen atmosphere, which resulted in the creation of the FePd:Cu alloy. The structure of alloy films obtained this way was determined by x-ray diffraction (XRD), glancing angle x-ray diffraction, and x-ray absorption fine structure (EXAFS). The measurements clearly showed that the L10 FePd:Cu nanocrystalline phase has been formed during the annealing process for all investigated copper compositions. This paper concentrates on the crystallographic grain features of FePd:Cu alloys and illustrates that the EXAFS technique, supported by XRD measurements, can help to extend the information about grain size and grain shape of poorly crystallized materials. We show that, using an appropriate model of the FePd:Cu grains, the comparison of EXAFS and XRD results gives a reasonable agreement.

Reactor for tracking catalyst nanoparticles in liquid at high temperature under a high-pressure gas phase with X-ray absorption spectroscopy.

PubMed

Nguyen, Luan; Tao, Franklin Feng

2018-02-01

Structure of catalyst nanoparticles dispersed in liquid phase at high temperature under gas phase of reactant(s) at higher pressure (≥5 bars) is important for fundamental understanding of catalytic reactions performed on these catalyst nanoparticles. Most structural characterizations of a catalyst performing catalysis in liquid at high temperature under gas phase at high pressure were performed in an ex situ condition in terms of characterizations before or after catalysis since, from technical point of view, access to the catalyst nanoparticles during catalysis in liquid phase at high temperature under high pressure reactant gas is challenging. Here we designed a reactor which allows us to perform structural characterization using X-ray absorption spectroscopy including X-ray absorption near edge structure spectroscopy and extended X-ray absorption fine structure spectroscopy to study catalyst nanoparticles under harsh catalysis conditions in terms of liquid up to 350 °C under gas phase with a pressure up to 50 bars. This reactor remains nanoparticles of a catalyst homogeneously dispersed in liquid during catalysis and X-ray absorption spectroscopy characterization.

X-RAYS FROM A RADIO-LOUD COMPACT BROAD ABSORPTION LINE QUASAR 1045+352 AND THE NATURE OF OUTFLOWS IN RADIO-LOUD BROAD ABSORPTION LINE QUASARS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kunert-Bajraszewska, Magdalena; Katarzynski, Krzysztof; Siemiginowska, Aneta

2009-11-10

We present new results on X-ray properties of radio-loud broad absorption line (BAL) quasars and focus on broadband spectral properties of a high-ionization BAL (HiBAL) compact steep spectrum (CSS) radio-loud quasar 1045+352. This HiBAL quasar has a very complex radio morphology indicating either strong interactions between a radio jet and the surrounding interstellar medium or a possible re-start of the jet activity. We detected 1045+352 quasar in a short 5 ksec Chandra ACIS-S observation. We applied theoretical models to explain spectral energy distribution of 1045+352 and argue that non-thermal, inverse-Compton (IC) emission from the innermost parts of the radio jetmore » can account for a large fraction of the observed X-ray emission. In our analysis, we also consider a scenario in which the observed X-ray emission from radio-loud BAL quasars can be a sum of IC jet X-ray emission and optically thin corona X-ray emission. We compiled a sample of radio-loud BAL quasars that were observed in X-rays to date and report no correlation between their X-ray and radio luminosity. However, the radio-loud BAL quasars show a large range of X-ray luminosities and absorption columns. This is consistent with the results obtained earlier for radio-quiet BAL quasars and may indicate an orientation effect in BAL quasars or more complex dependence between X-ray emission, radio emission, and an orientation based on the radio morphology.« less

Structural analysis of nanocrystalline ZnTe alloys synthesized by melt quenching technique

NASA Astrophysics Data System (ADS)

Singh, Harinder; Singh, Tejbir; Thakur, Anup; Sharma, Jeewan

2018-05-01

Nanocrystalline ZnxTe100-x (x=0, 5, 20, 30, 40, 50) alloys have been synthesized using melt quenching technique. Energy-dispersive X-Ray spectroscopy (EDS) has been used to verify the elemental composition of samples. Various absorption modes are recorded from Fourier transform infrared spectroscopy (FTIR) confirming the formation of ZnTe. The structural study has been performed using X-Ray Diffraction (XRD) method. All synthesized samples have been found to be nanocrystalline in nature with average crystallite size in the range from 49.3 nm to 77.1 nm. Results have shown that Zn0Te100 exhibits hexagonal phase that transforms into a cubic ZnTe phase as the amount of zinc is increased. Pure ZnTe phase has been obtained for x = 50. The texture coefficient (Tc) has been calculated to find the prominent orientations of different planes.

Comparative Analysis of Microbial Communities in Iron-Dominated Flocculent Mats in Deep-Sea Hydrothermal Environments

PubMed Central

Kikuchi, Sakiko; Mitsunobu, Satoshi; Takaki, Yoshihiro; Yamanaka, Toshiro; Toki, Tomohiro; Noguchi, Takuroh; Nakamura, Kentaro; Abe, Mariko; Hirai, Miho; Yamamoto, Masahiro; Uematsu, Katsuyuki; Miyazaki, Junichi; Nunoura, Takuro; Takahashi, Yoshio; Takai, Ken

2016-01-01

ABSTRACT It has been suggested that iron is one of the most important energy sources for photosynthesis-independent microbial ecosystems in the ocean crust. Iron-metabolizing chemolithoautotrophs play a key role as primary producers, but little is known about their distribution and diversity and their ecological role as submarine iron-metabolizing chemolithotrophs, particularly the iron oxidizers. In this study, we investigated the microbial communities in several iron-dominated flocculent mats found in deep-sea hydrothermal fields in the Mariana Volcanic Arc and Trough and the Okinawa Trough by culture-independent molecular techniques and X-ray mineralogical analyses. The abundance and composition of the 16S rRNA gene phylotypes demonstrated the ubiquity of zetaproteobacterial phylotypes in iron-dominated mat communities affected by hydrothermal fluid input. Electron microscopy with energy-dispersive X-ray microanalysis and X-ray absorption fine structure (XAFS) analysis revealed the chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species and the potential contribution of Zetaproteobacteria to the in situ generation. These results suggest that putative iron-oxidizing chemolithoautotrophs play a significant ecological role in producing iron-dominated flocculent mats and that they are important for iron and carbon cycles in deep-sea low-temperature hydrothermal environments. IMPORTANCE We report novel aspects of microbiology from iron-dominated flocculent mats in various deep-sea environments. In this study, we examined the relationship between Zetaproteobacteria and iron oxides across several hydrothermally influenced sites in the deep sea. We analyzed iron-dominated mats using culture-independent molecular techniques and X-ray mineralogical analyses. The scanning electron microscopy–energy-dispersive X-ray spectroscopy SEM-EDS analysis and X-ray absorption fine structure (XAFS) analysis revealed chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species as well as the potential contribution of the zetaproteobacterial population to the in situ production. These key findings provide important information for understanding the mechanisms of both geomicrobiological iron cycling and the formation of iron-dominated mats in deep-sea hydrothermal fields. PMID:27422841

Detailed Characterization of a Nanosecond-Lived Excited State: X-ray and Theoretical Investigation of the Quintet State in Photoexcited [Fe(terpy)2]2+

PubMed Central

2015-01-01

Theoretical predictions show that depending on the populations of the Fe 3dxy, 3dxz, and 3dyz orbitals two possible quintet states can exist for the high-spin state of the photoswitchable model system [Fe(terpy)2]2+. The differences in the structure and molecular properties of these 5B2 and 5E quintets are very small and pose a substantial challenge for experiments to resolve them. Yet for a better understanding of the physics of this system, which can lead to the design of novel molecules with enhanced photoswitching performance, it is vital to determine which high-spin state is reached in the transitions that follow the light excitation. The quintet state can be prepared with a short laser pulse and can be studied with cutting-edge time-resolved X-ray techniques. Here we report on the application of an extended set of X-ray spectroscopy and scattering techniques applied to investigate the quintet state of [Fe(terpy)2]2+ 80 ps after light excitation. High-quality X-ray absorption, nonresonant emission, and resonant emission spectra as well as X-ray diffuse scattering data clearly reflect the formation of the high-spin state of the [Fe(terpy)2]2+ molecule; moreover, extended X-ray absorption fine structure spectroscopy resolves the Fe–ligand bond-length variations with unprecedented bond-length accuracy in time-resolved experiments. With ab initio calculations we determine why, in contrast to most related systems, one configurational mode is insufficient for the description of the low-spin (LS)–high-spin (HS) transition. We identify the electronic structure origin of the differences between the two possible quintet modes, and finally, we unambiguously identify the formed quintet state as 5E, in agreement with our theoretical expectations. PMID:25838847

Detailed Characterization of a Nanosecond-Lived Excited State: X-ray and Theoretical Investigation of the Quintet State in Photoexcited [Fe(terpy) 2 ] 2+

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vankó, György; Bordage, Amélie; Pápai, Mátyás

2015-03-19

Theoretical predictions show that depending on the populations of the Fe 3dxy, 3dxz, and 3dyz orbitals two possible quintet states can exist for the high-spin state of the photoswitchable model system [Fe(terpy)2]2+. The differences in the structure and molecular properties of these 5B2 and 5E quintets are very small and pose a substantial challenge for experiments to resolve them. Yet for a better understanding of the physics of this system, which can lead to the design of novel molecules with enhanced photoswitching performance, it is vital to determine which high-spin state is reached in the transitions that follow the lightmore » excitation. The quintet state can be prepared with a short laser pulse and can be studied with cutting-edge time-resolved X-ray techniques. Here we report on the application of an extended set of X-ray spectroscopy and scattering techniques applied to investigate the quintet state of [Fe(terpy)2]2+ 80 ps after light excitation. High-quality X-ray absorption, nonresonant emission, and resonant emission spectra as well as X-ray diffuse scattering data clearly reflect the formation of the high-spin state of the [Fe(terpy)2]2+ molecule; moreover, extended X-ray absorption fine structure spectroscopy resolves the Fe-ligand bond-length variations with unprecedented bondlength accuracy in time-resolved experiments. With ab initio calculations we determine why, in contrast to most related systems, one configurational mode is insufficient for the description of the low-spin (LS)-high-spin (HS) transition. We identify the electronic structure origin of the differences between the two possible quintet modes, and finally, we unambiguously identify the formed quintet state as 5E, in agreement with our theoretical expectations.« less

Detailed Characterization of a Nanosecond-Lived Excited State: X-ray and Theoretical Investigation of the Quintet State in Photoexcited [Fe(terpy) 2 ] 2+

DOE PAGES

Vanko, Gyorgy; Bordage, Amelie; Papai, Matyas; ...

2015-03-19

Theoretical predictions show that depending on the populations of the Fe 3d xy, 3d xz, and 3d yz orbitals two possible quintet states can exist for the high-spin state of the photoswitchable model system [Fe(terpy) 2] 2+. The differences in the structure and molecular properties of these 5B2 and 5E quintets are very small and pose a substantial challenge for experiments to resolve them. Yet for a better understanding of the physics of this system, which can lead to the design of novel molecules with enhanced photoswitching performance, it is vital to determine which high-spin state is reached in themore » transitions that follow the light excitation. The quintet state can be prepared with a short laser pulse and can be studied with cutting-edge time-resolved X-ray techniques. Here we report on the application of an extended set of X-ray spectroscopy and scattering techniques applied to investigate the quintet state of [Fe(terpy) 2] 2+ 80 ps after light excitation. High-quality X-ray absorption, nonresonant emission, and resonant emission spectra as well as X-ray diffuse scattering data clearly reflect the formation of the high-spin state of the [Fe(terpy) 2] 2+ molecule; moreover, extended X-ray absorption fine structure spectroscopy resolves the Fe–ligand bond-length variations with unprecedented bond-length accuracy in time-resolved experiments. With ab initio calculations we determine why, in contrast to most related systems, one configurational mode is insufficient for the description of the low-spin (LS)–high-spin (HS) transition. We identify the electronic structure origin of the differences between the two possible quintet modes, and finally, we unambiguously identify the formed quintet state as 5E, in agreement with our theoretical expectations.« less

Ultrapressure materials science

NASA Technical Reports Server (NTRS)

Ruoff, A. L.

1984-01-01

Three active areas of research at ultra pressure are pursued, i.e., diffraction studies with the Cornell High Energy Synchrotron Source (CHESS), band gap and absorption edge effects, indentor-anvil experiments and theory and research to attain higher pressures. The range over which X-ray diffraction data and absorption edge data are obtained is extended to 700 kbars. Using the indentor technique pressures of 2.1 Mbars are obtained. Research results and methods are discussed.

A comparison of two micro-beam X-ray emission techniques for actinide elemental distribution in microscopic particles originating from the hydrogen bombs involved in the Palomares (Spain) and Thule (Greenland) accidents

NASA Astrophysics Data System (ADS)

Jimenez-Ramos, M. C.; Eriksson, M.; García-López, J.; Ranebo, Y.; García-Tenorio, R.; Betti, M.; Holm, E.

2010-09-01

In order to validate and to gain confidence in two micro-beam techniques: particle induced X-ray emission with nuclear microprobe technique (μ-PIXE) and synchrotron radiation induced X-ray fluorescence in a confocal alignment (confocal SR μ-XRF) for characterization of microscopic particles containing actinide elements (mixed plutonium and uranium) a comparative study has been performed. Inter-comparison of the two techniques is essential as the X-ray production cross-sections for U and Pu are different for protons and photons and not well defined in the open literature, especially for Pu. The particles studied consisted of nuclear weapons material, and originate either in the so called Palomares accident in Spain, 1966 or in the Thule accident in Greenland, 1968. In the determination of the average Pu/U mass ratios (not corrected by self-absorption) in the analysed microscopic particles the results from both techniques show a very good agreement. In addition, the suitability of both techniques for the analysis with good resolution (down to a few μm) of the Pu/U distribution within the particles has been proved. The set of results obtained through both techniques has allowed gaining important information concerning the characterization of the remaining fissile material in the areas affected by the aircraft accidents. This type of information is essential for long-term impact assessments of contaminated sites.

X-ray Absorption Spectroscopy Characterization of a Li/S Cell

DOE PAGES

Ye, Yifan; Kawase, Ayako; Song, Min-Kyu; ...

2016-01-11

The X-ray absorption spectroscopy technique has been applied to study different stages of the lithium/sulfur (Li/S) cell life cycle. We investigated how speciation of S in Li/S cathodes changes upon the introduction of CTAB (cetyltrimethylammonium bromide, CH 3(CH 2) 15N+(CH 3) 3Br₋) and with charge/discharge cycling. The introduction of CTAB changes the synthesis reaction pathway dramatically due to the interaction of CTAB with the terminal S atoms of the polysulfide ions in the Na 2S x solution. For the cycled Li/S cell, the loss of electrochemically active sulfur and the accumulation of a compact blocking insulating layer of unexpected sulfurmore » reaction products on the cathode surface during the charge/discharge processes make the capacity decay. Lastly, a modified coin cell and a vacuum-compatible three-electrode electro-chemical cell have been introduced for further in-situ/in-operando studies.« less

X-Ray Microanalysis and Electron Energy Loss Spectrometry in the Analytical Electron Microscope: Review and Future Directions

NASA Technical Reports Server (NTRS)

Goldstein, J. I.; Williams, D. B.

1992-01-01

This paper reviews and discusses future directions in analytical electron microscopy for microchemical analysis using X-ray and Electron Energy Loss Spectroscopy (EELS). The technique of X-ray microanalysis, using the ratio method and k(sub AB) factors, is outlined. The X-ray absorption correction is the major barrier to the objective of obtaining I% accuracy and precision in analysis. Spatial resolution and Minimum Detectability Limits (MDL) are considered with present limitations of spatial resolution in the 2 to 3 microns range and of MDL in the 0.1 to 0.2 wt. % range when a Field Emission Gun (FEG) system is used. Future directions of X-ray analysis include improvement in X-ray spatial resolution to the I to 2 microns range and MDL as low as 0.01 wt. %. With these improvements the detection of single atoms in the analysis volume will be possible. Other future improvements include the use of clean room techniques for thin specimen preparation, quantification available at the I% accuracy and precision level with light element analysis quantification available at better than the 10% accuracy and precision level, the incorporation of a compact wavelength dispersive spectrometer to improve X-ray spectral resolution, light element analysis and MDL, and instrument improvements including source stability, on-line probe current measurements, stage stability, and computerized stage control. The paper reviews the EELS technique, recognizing that it has been slow to develop and still remains firmly in research laboratories rather than in applications laboratories. Consideration of microanalysis with core-loss edges is given along with a discussion of the limitations such as specimen thickness. Spatial resolution and MDL are considered, recognizing that single atom detection is already possible. Plasmon loss analysis is discussed as well as fine structure analysis. New techniques for energy-loss imaging are also summarized. Future directions in the EELS technique will be the development of new spectrometers and improvements in thin specimen preparation. The microanalysis technique needs to be simplified and software developed so that the EELS technique approaches the relative simplicity of the X-ray technique. Finally, one can expect major improvements in EELS imaging as data storage and processing improvements occur.

A dual-PIXE tomography setup for reconstruction of Germanium in ICF target

NASA Astrophysics Data System (ADS)

Guo, N.; Lu, H. Y.; Wang, Q.; Meng, J.; Gao, D. Z.; Zhang, Y. J.; Liang, X. X.; Zhang, W.; Li, J.; Ma, X. J.; Shen, H.

2017-08-01

Inertial Confinement Fusion (ICF) is one type of fusion energy research which could initiate nuclear fusion reactions through heating and compressing thermonuclear fuel. Compared to a pure plastic target, Germanium doping into the CH ablator layer by Glow Discharge Polymer (GDP) technique can increase the ablation velocity and the standoff distance between the ablation front and laser-deposition region. During target fabrication process, quantitative doping of Ge should be accurately controlled. Particle Induced X-ray Emission Tomography (PIXE-T) can make not only quantification of the concentration, but also reconstruction of the spatial distribution of doped element. The Si (Li) detector for PIXE tomography technique had a disadvantage of low counting rate. To make up this deficiency, another detector of Si (Li) with the same configuration positioned at the opposite side with the same detective angle 135° have been implemented. Simultaneously acquired elemental maps of Ge obtained using two detectors may be different because of the X-ray absorption along the X-ray exit route in the target. In this paper, the X-ray detection efficiency is drastically improved by this dual-PIXE tomography system.

Thomson Thick X-Ray Absorption in a Broad Absorption Line Quasar, PG 0946+301.

PubMed

Mathur; Green; Arav; Brotherton; Crenshaw; deKool; Elvis; Goodrich; Hamann; Hines; Kashyap; Korista; Peterson; Shields; Shlosman; van Breugel W; Voit

2000-04-20

We present a deep ASCA observation of a broad absorption line quasar (BALQSO) PG 0946+301. The source was clearly detected in one of the gas imaging spectrometers, but not in any other detector. If BALQSOs have intrinsic X-ray spectra similar to normal radio-quiet quasars, our observations imply that there is Thomson thick X-ray absorption (NH greater, similar1024 cm-2) toward PG 0946+301. This is the largest column density estimated so far toward a BALQSO. The absorber must be at least partially ionized and may be responsible for attenuation in the optical and UV. If the Thomson optical depth toward BALQSOs is close to 1, as inferred here, then spectroscopy in hard X-rays with large telescopes like XMM would be feasible.

Thermal effects on the structural properties of tungsten oxide nanoparticles

NASA Astrophysics Data System (ADS)

Yang, Tsung-Yeh; Wu, Chung-Yi; Tsai, Meng-Hung; Lin, Hong-Ming; Tsai, Wen-Li; Hwu, Yeukuang

2004-06-01

Tungsten oxide nanoparticles are prepared by evaporating and oxidizing the tungsten boat in helium and oxygen atmosphere and then quenched to the liquid nitrogen temperature. The as-prepared tungsten oxide nanoparticles are porous-free with uniform size. The morphology and particle size distribution of the as-prepared and after sinter treatments tungsten oxide nanoparticles are revealed by TEM and AFM. The long-range order of these nanoparticles can be examined by X-ray diffraction technique. The as-prepared nanoparticles exhibit a mixture structure of monoclinic and hexagonal crystals. Preliminary X-ray diffraction results indicate that the hexagonal structure is transformed to monoclinic structure after annealing to above 600°C. In order to better distinguish the structural properties of the tungsten oxide (WO3- x) nanoparticles before and after annealing, the X-ray absorption spectrum technique is utilized; thus, the detailed local atomic arrangement of oxygen and/or tungsten can be determined. According to the XAS result, the shape of the W L3-edge undergoes no considerable changes. This infers that structural transformation of tungsten oxide nanoparticle may be caused by the migration of oxygen after sintering. From the O K-edge of absorption spectrum, it suggests that a mixture phase structure is obtained when sintered below 300°C. And this result indicates that heat treatment to approximately 600°C produces a stable structure of a monoclinic crystal of WO3.

Measuring the Dust Grains and Distance to X Persei Via Its X-ray Halo

NASA Astrophysics Data System (ADS)

Smith, Randall

2006-09-01

We propose to observe the X-ray halo of the high mass X-ray binary pulsar X Per to measure interstellar dust grains along the line of sight (LOS) and to determine the distance to X Per. The X-ray halo is formed by scattering from grains along the LOS, which for X Per appear to be concentrated in one molecular cloud. Unlike many other X-ray halo observations, this low-absorption high-latitude sightline is well-characterized from absorption spectroscopy done with HST, Copernicus, and FUSE. This halo observation will measure the distance to the cloud and the dust size distribution in it. We will also be able to determine the distance to X Per by measuring the time delayed pulses in the X-ray halo.

Microanalysis of iron oxidation state in iron oxides using X Ray Absorption Near Edge Structure (XANES)

NASA Technical Reports Server (NTRS)

Sutton, S. R.; Delaney, J.; Bajt, S.; Rivers, M. L.; Smith, J. V.

1993-01-01

An exploratory application of x ray absorption near edge structure (XANES) analysis using the synchrotron x ray microprobe was undertaken to obtain Fe XANES spectra on individual sub-millimeter grains in conventional polished sections. The experiments concentrated on determinations of Fe valence in a suite of iron oxide minerals for which independent estimates of the iron speciation could be made by electron microprobe analysis and x ray diffraction.

Comprehensive Experimental and Computational Spectroscopic Study of Hexacyanoferrate Complexes in Water: From Infrared to X-ray Wavelengths.

PubMed

Ross, Matthew; Andersen, Amity; Fox, Zachary W; Zhang, Yu; Hong, Kiryong; Lee, Jae-Hyuk; Cordones, Amy; March, Anne Marie; Doumy, Gilles; Southworth, Stephen H; Marcus, Matthew A; Schoenlein, Robert W; Mukamel, Shaul; Govind, Niranjan; Khalil, Munira

2018-05-17

We present a joint experimental and computational study of the hexacyanoferrate aqueous complexes at equilibrium in the 250 meV to 7.15 keV regime. The experiments and the computations include the vibrational spectroscopy of the cyanide ligands, the valence electronic absorption spectra, and Fe 1s core hole spectra using element-specific-resonant X-ray absorption and emission techniques. Density functional theory-based quantum mechanics/molecular mechanics molecular dynamics simulations are performed to generate explicit solute-solvent configurations, which serve as inputs for the spectroscopy calculations of the experiments spanning the IR to X-ray wavelengths. The spectroscopy simulations are performed at the same level of theory across this large energy window, which allows for a systematic comparison of the effects of explicit solute-solvent interactions in the vibrational, valence electronic, and core-level spectra of hexacyanoferrate complexes in water. Although the spectroscopy of hexacyanoferrate complexes in solution has been the subject of several studies, most of the previous works have focused on a narrow energy window and have not accounted for explicit solute-solvent interactions in their spectroscopy simulations. In this work, we focus our analysis on identifying how the local solvation environment around the hexacyanoferrate complexes influences the intensity and line shape of specific spectroscopic features in the UV/vis, X-ray absorption, and valence-to-core X-ray emission spectra. The identification of these features and their relationship to solute-solvent interactions is important because hexacyanoferrate complexes serve as model systems for understanding the photochemistry and photophysics of a large class of Fe(II) and Fe(III) complexes in solution.

High-resolution x-ray absorption spectroscopy studies of metal compounds in neurodegenerative brain tissue

NASA Astrophysics Data System (ADS)

Collingwood, J. F.; Mikhaylova, A.; Davidson, M. R.; Batich, C.; Streit, W. J.; Eskin, T.; Terry, J.; Barrea, R.; Underhill, R. S.; Dobson, J.

2005-01-01

Fluorescence mapping and microfocus X-ray absorption spectroscopy are used to detect, locate and identify iron biominerals and other inorganic metal accumulations in neurodegenerative brain tissue at sub-cellular resolution (<5 microns). Recent progress in developing the technique is reviewed. Synchrotron X-rays are used to map tissue sections for metals of interest, and XANES and XAFS are used to characterise anomalous concentrations of the metals in-situ so that they can be correlated with tissue structures and disease pathology. Iron anomalies associated with biogenic magnetite, ferritin and haemoglobin are located and identified in an avian tissue model with a pixel resolution ~5 microns. Subsequent studies include brain tissue sections from transgenic Huntington's mice, and the first high-resolution mapping and identification of iron biominerals in human Alzheimer's and control autopsy brain tissue. Technical developments include use of microfocus diffraction to obtain structural information about biominerals in-situ, and depositing sample location grids by lithography for the location of anomalies by conventional microscopy. The combined techniques provide a breakthrough in the study of both intra- and extra-cellular iron compounds and related metals in tissue. The information to be gained from this approach has implications for future diagnosis and treatment of neurodegeneration, and for our understanding of the mechanisms involved.

Time-Resolved X-Ray Magnetic Circular Dichroism - A Selective Probe of Magnetization Dynamics on Nanosecond Timescales

NASA Astrophysics Data System (ADS)

Pizzini, Stefania; Vogel, Jan; Bonfim, Marlio; Fontaine, Alain

Many synchrotron radiation techniques have been developed in the last 15 years for studying the magnetic properties of thin-film materials. The most attractive properties of synchrotron radiation are its energy tunability and its time structure. The first property allows measurements in resonant conditions at an absorption edge of each of the magnetic elements constituting the probed sample, and the latter allows time-resolved measurements on subnanosecond timescales. In this review, we introduce some of the synchrotron-based techniques used for magnetic investigations. We then describe in detail X-ray magnetic circular dichroism (XMCD) and how time-resolved XMCD studies can be carried out in the pump-probe mode. Finally, we illustrate some applications to magnetization reversal dynamics in spin valves and tunnel junctions, using fast magnetic field pulses applied along the easy magnetization axis of the samples. Thanks to the element-selectivity of X-ray absorption spectroscopy, the magnetization dynamics of the soft (Permalloy) and the hard (cobalt) layers can be studied independently. In the case of spin valves, this allowed us to show that two magnetic layers that are strongly coupled in a static regime can become uncoupled on nanosecond timescales.Present address: Universidade Federal do Paraná, Centro Politécnico CP 19011, Curitiba - PR CEP 81531-990, Brazil

Elemental and Molecular Segregation in Oil Paintings due to Lead Soap Degradation.

PubMed

Chen-Wiegart, Yu-Chen Karen; Catalano, Jaclyn; Williams, Garth J; Murphy, Anna; Yao, Yao; Zumbulyadis, Nicholas; Centeno, Silvia A; Dybowski, Cecil; Thieme, Juergen

2017-09-14

The formation of Pb, Zn, and Cu carboxylates (soaps) has caused visible deterioration in hundreds of oil paintings dating from the 15th century to the present. Through transport phenomena not yet understood, free fatty acids in the oil binding medium migrate through the paint and react with pigments containing heavy metals to form soaps. To investigate the complex correlation among the elemental segregation, types of chemical compounds formed, and possible mechanisms of the reactions, a paint sample cross-section from a 15th century oil painting was examined by synchrotron X-ray techniques. X-ray fluorescence (XRF) microscopy, quantified with elemental correlation density distribution, showed Pb and Sn segregation in the soap-affected areas. X-ray absorption near edge structure (XANES) around the Pb-L3 absorption edge showed that Pb pigments and Pb soaps can be distinguished while micro-XANES gave further information on the chemical heterogeneity in the paint film. The advantages and limitations of these synchrotron-based techniques are discussed and compared to those of methods routinely used to analyze paint samples. The results presented set the stage for improving the information extracted from samples removed from works of art and for correlating observations in model paint samples to those in the naturally aged samples, to shed light onto the mechanism of soap formation.

Lithographically fabricated silicon microreactor for in situ characterization of heterogeneous catalysts—Enabling correlative characterization techniques

NASA Astrophysics Data System (ADS)

Baier, S.; Rochet, A.; Hofmann, G.; Kraut, M.; Grunwaldt, J.-D.

2015-06-01

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The silicon microreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy. Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor for in situ studies.

Lithographically fabricated silicon microreactor for in situ characterization of heterogeneous catalysts—Enabling correlative characterization techniques.

PubMed

Baier, S; Rochet, A; Hofmann, G; Kraut, M; Grunwaldt, J-D

2015-06-01

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The silicon microreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy. Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor for in situ studies.

Melting of iron determined by X-ray absorption spectroscopy to 100 GPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aquilanti, Giuliana; Trapananti, Angela; Karandikar, Amol

2015-09-14

There is a long-standing controversy over the melting curve of Fe at high pressure as determined from static laser heated diamond anvil cell and dynamic compression studies. X-ray absorption spectroscopy measurements are used here as a criterion to detect melting under pressure. Confronted with a diversity of obtained melting curves, this technique, used at such pressure and temperature conditions, is eligible to be at the forefront to probe Earth's deep interior. Furthermore, the experiment reported here holds promise for addressing important issues related to the structure and phase diagram of compressed melts, such as the existence of structural complexity (polyamorphism)more » in the liquid phase or the extent of icosahedral ordering whose investigation has been limited until now to ambient conditions.« less

Ordered Self-Assembled Monolayers of Peptide Nucleic Acids with DNA Recognition Capability

NASA Astrophysics Data System (ADS)

Briones, C.; Mateo-Marti, E.; Gómez-Navarro, C.; Parro, V.; Román, E.; Martín-Gago, J. A.

2004-11-01

We report on the formation of ordered self-assembled monolayers (SAMs) of single-stranded peptide nucleic acids (ssPNA). In spite of their remarkable length (7nm) thiolated PNAs assemble standing up on gold surfaces similarly to the SAMs of short alkanethiols. SAMs of ssPNA recognize complementary nucleic acids, acting as specific biosensors that discriminate even a point mutation in target ssDNA. These results are obtained by surface characterization techniques that avoid labeling of the target molecule: x-ray photoemission, x-ray absorption and atomic force microscopy.

X-ray absorption spectroscopy investigations on oxidized Ni/Au contacts to p-GaN.

PubMed

Jan, J C; Asokan, K; Chiou, J W; Pong, W F; Tseng, P K; Chen, L C; Chen, F R; Lee, J F; Wu, J S; Lin, H J; Chen, C T

2001-03-01

X-ray absorption spectroscopy was used to investigate the electronic structure of as-deposited and oxidized Ni/Au contacts to p-GaN and to elucidate the mechanism responsible for low impedance. X-ray absorption near edge spectra of Ni K- and L3,2-edges clearly indicate formation of NiO on the sample surface after annealing. The reason for low impedance may be attributed to increase in hole concentration and existence of p-NiO layer on the surface.

Studies by Near Edge X-ray Absorption Spectroscopies of Bonding Dynamics at the Graphene/Guanine Interface - A Proposal for High Mobility, Organic Graphene Field Effect Transistors

DTIC Science & Technology

2015-07-01

AFRL-AFOSR-UK-TR-2015-0034 Studies by Near Edge X-ray Absorption Spectroscopies of Bonding Dynamics at the Graphene /Guanine...Interface – A Proposal for High Mobility, Organic Graphene Field Effect Transistors Eva Campo BANGOR UNIVERSITY COLLEGE ROAD BANGOR...April 2015 4. TITLE AND SUBTITLE Studies by Near Edge X-ray Absorption Spectroscopies of Bonding Dynamics at the Graphene /Guanine Interface - A

Search for correlated UV and x ray absorption of NGC 3516

NASA Technical Reports Server (NTRS)

Martin, Christopher; Halpern, Jules P.; Kolman, Michiel

1991-01-01

NGC 3516, a low-luminosity Seyfert galaxy, is one of a small fraction of Seyfert galaxies that exhibit broad absorption in a resonance line. In order to determine whether the UV and x ray absorption in NGC 3516 are related, 5 IUE observations were obtained, quasi-simultaneously with 4 Ginga observations. The results are presented and discussed. The following subject areas are covered: short-term UV variability; emission lines; galactic absorption lines; the C IV, N V, and Si IV absorption features; lower limit on the carbon column density; estimate of the distance from the absorber to the continuum source; variability in the continuum and absorption; a comparison with BAL QSO's; and the x ray-UV connection.

Examination of Arsenic Speciation in Sulfidic Solutions Using X-ray Absorption Spectroscopy

EPA Science Inventory

The chemical speciation of arsenic in sulfidic waters is complicated by the existence of thioarsenic species. The purpose of this research was to use advanced spectroscopy techniques along with speciation modeling and chromatography to elucidate the chemical speciation of As in ...

Legacy phosphorus in calcareous soils: Effects of long-term poultry litter application

USDA-ARS?s Scientific Manuscript database

The effect of manure application on soil phosphorus has been intensively studied with modifications of the Hedley sequential fractionation procedure, X ray absorption near edge structure spectroscopy, and 31P nuclear magnetic resonance. Modern sequential fractionation techniques, coupled with phosph...

Near-edge x-ray absorption fine structure spectroscopy at atmospheric pressure with a table-top laser-induced soft x-ray source

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kühl, Frank-Christian, E-mail: Frank-christian.kuehl@mail.de; Müller, Matthias, E-mail: matthias.mueller@llg-ev.de; Schellhorn, Meike

2016-07-15

The authors present a table-top soft x-ray absorption spectrometer, accomplishing investigations of the near-edge x-ray absorption fine structure (NEXAFS) in a laboratory environment. The system is based on a low debris plasma ignited by a picosecond laser in a pulsed krypton gas jet, emitting soft x-ray radiation in the range from 1 to 5 nm. For absorption spectroscopy in and around the “water window” (2.3–4.4 nm), a compact helium purged sample compartment for experiments at atmospheric pressure has been constructed and tested. NEXAFS measurements on CaCl{sub 2} and KMnO{sub 4} samples were conducted at the calcium and manganese L-edges, as well asmore » at the oxygen K-edge in air, atmospheric helium, and under vacuum, respectively. The results indicate the importance of atmospheric conditions for an investigation of sample hydration processes.« less

The Soft X-ray View of Ultra Fast Outflows

NASA Astrophysics Data System (ADS)

Reeves, J.; Braito, V.; Nardini, E.; Matzeu, G.; Lobban, A.; Costa, M.; Pounds, K.; Tombesi, F.; Behar, E.

2017-10-01

The recent large XMM-Newton programmes on the nearby quasars PDS 456 and PG 1211+143 have revealed prototype ultra fast outflows in the iron K band through highly blue shifted absorption lines. The wind velocities are in excess of 0.1c and are likely to make a significant contribution to the host galaxy feedback. Here we present evidence for the signature of the fast wind in the soft X-ray band from these luminous quasars, focusing on the spectroscopy with the RGS. In PDS 456, the RGS spectra reveal the presence of soft X-ray broad absorption line profiles, which suggests that PDS 456 is an X-ray equivalent to the BAL quasars, with outflow velocities reaching 0.2c. In PG 1211, the soft X-ray RGS spectra show a complex of several highly blue shifted absorption lines over a wide range of ionisation and reveal outflowing components with velocities between 0.06-0.17c. For both quasars, the soft X-ray absorption is highly variable, even on timescales of days and is most prominent when the quasar flux is low. Overall the results imply the presence of a soft X-ray component of the ultra fast outflows, which we attribute to a clumpy or inhomogeneous phase of the disk wind.

Tracking ink composition on Herculaneum papyrus scrolls: quantification and speciation of lead by X-ray based techniques and Monte Carlo simulations

PubMed Central

Tack, Pieter; Cotte, Marine; Bauters, Stephen; Brun, Emmanuel; Banerjee, Dipanjan; Bras, Wim; Ferrero, Claudio; Delattre, Daniel; Mocella, Vito; Vincze, Laszlo

2016-01-01

The writing in carbonized Herculaneum scrolls, covered and preserved by the pyroclastic events of the Vesuvius in 79 AD, was recently revealed using X-ray phase-contrast tomography, without the need of unrolling the sensitive scrolls. Unfortunately, some of the text is difficult to read due to the interference of the papyrus fibers crossing the written text vertically and horizontally. Recently, lead was found as an elemental constituent in the writing, rendering the text more clearly readable when monitoring the lead X-ray fluorescence signal. Here, several hypotheses are postulated for the origin and state of lead in the papyrus writing. Multi-scale X-ray fluorescence micro-imaging, Monte Carlo quantification and X-ray absorption microspectroscopy experiments are used to provide additional information on the ink composition, in an attempt to determine the origin of the lead in the Herculaneum scrolls and validate the postulated hypotheses. PMID:26854067

Visualizing the non-equilibrium dynamics of photoinduced intramolecular electron transfer with femtosecond X-ray pulses

PubMed Central

Canton, Sophie E.; Kjær, Kasper S.; Vankó, György; van Driel, Tim B.; Adachi, Shin-ichi; Bordage, Amélie; Bressler, Christian; Chabera, Pavel; Christensen, Morten; Dohn, Asmus O.; Galler, Andreas; Gawelda, Wojciech; Gosztola, David; Haldrup, Kristoffer; Harlang, Tobias; Liu, Yizhu; Møller, Klaus B.; Németh, Zoltán; Nozawa, Shunsuke; Pápai, Mátyás; Sato, Tokushi; Sato, Takahiro; Suarez-Alcantara, Karina; Togashi, Tadashi; Tono, Kensuke; Uhlig, Jens; Vithanage, Dimali A.; Wärnmark, Kenneth; Yabashi, Makina; Zhang, Jianxin; Sundström, Villy; Nielsen, Martin M.

2015-01-01

Ultrafast photoinduced electron transfer preceding energy equilibration still poses many experimental and conceptual challenges to the optimization of photoconversion since an atomic-scale description has so far been beyond reach. Here we combine femtosecond transient optical absorption spectroscopy with ultrafast X-ray emission spectroscopy and diffuse X-ray scattering at the SACLA facility to track the non-equilibrated electronic and structural dynamics within a bimetallic donor–acceptor complex that contains an optically dark centre. Exploiting the 100-fold increase in temporal resolution as compared with storage ring facilities, these measurements constitute the first X-ray-based visualization of a non-equilibrated intramolecular electron transfer process over large interatomic distances. Experimental and theoretical results establish that mediation through electronically excited molecular states is a key mechanistic feature. The present study demonstrates the extensive potential of femtosecond X-ray techniques as diagnostics of non-adiabatic electron transfer processes in synthetic and biological systems, and some directions for future studies, are outlined. PMID:25727920

Visualizing the non-equilibrium dynamics of photoinduced intramolecular electron transfer with femtosecond X-ray pulses

DOE PAGES

Canton, Sophie E.; Kjær, Kasper S.; Vankó, György; ...

2015-03-02

Ultrafast photoinduced electron transfer preceding energy equilibration still poses many experimental and conceptual challenges to the optimization of photoconversion since an atomic-scale description has so far been beyond reach. Here we combine femtosecond transient optical absorption spectroscopy with ultrafast X-ray emission spectroscopy and diffuse X-ray scattering at the SACLA facility to track the non-equilibrated electronic and structural dynamics within a bimetallic donor–acceptor complex that contains an optically dark centre. Exploiting the 100-fold increase in temporal resolution as compared with storage ring facilities, these measurements constitute the first X-ray-based visualization of a non-equilibrated intramolecular electron transfer process over large interatomic distances.more » Thus experimental and theoretical results establish that mediation through electronically excited molecular states is a key mechanistic feature. The present study demonstrates the extensive potential of femtosecond X-ray techniques as diagnostics of non-adiabatic electron transfer processes in synthetic and biological systems, and some directions for future studies, are outlined.« less

X-ray Reflectivity Characterization of Ion Distribution at Biomimetic Membrane Surfaces

NASA Astrophysics Data System (ADS)

Krüger, Peter; Pittler, Jens; Vaknin, David; Lösche, Mathias

2003-03-01

Ions at cell membrane surfaces may control the function and conformation of nearby biomolecules, thus playing an important role in inter- and intracellular transport as well as in biorecognition processes. Moreover, charge patterns at membrane surfaces may direct the growth of inorganic crystals in biomineralization. Langmuir monolayers are widely employed as model systems for studying charge distribution and growth processes at the organic/inorganic interface. We present a novel x-ray reflectivity technique that provides detailed information on ion distribution at biomembrane surfaces by using monochromatic x-rays at various energies at and away from the ion x-ray absorption edges. As a model, the interaction of Ba^2+ with DMPA^- (dimyristoyl phosphatidic acid) monolayers at the aqueous surface was studied. We find an unexpectedly large concentration of the cations near the interface where they form a Stern layer of bound ions. These studies have been complemented with conventional x-ray reflectivity measurements and extended to other anionic lipid species (DMPS, DMPG) and cations (Ca^2+).

An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

NASA Technical Reports Server (NTRS)

Ross, H. Richard

1993-01-01

A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

Direct X-ray detection with hybrid solar cells based on organolead halide perovskites

NASA Astrophysics Data System (ADS)

Gill, Hardeep Singh; Elshahat, Bassem; Sajo, Erno; Kumar, Jayant; Kokil, Akshay; Zygmanski, Piotr; Li, Lian; Mosurkal, Ravi

2014-03-01

Organolead halide perovskite materials are attracting considerable interest due to their exceptional opto-electronic properties, such as, high charge carrier mobilities, high exciton diffusion length, high extinction coefficients and broad-band absorption. These interesting properties have enabled their application in high performance hybrid photovoltaic devices. The high Z value of their constituents also makes these materials efficient for absorbing X-rays. Here we will present on the efficient use of hybrid solar cells based on organolead perovskite materials as X-ray detectors. Hybrid solar cells based on CH3NH3PbI3 were fabricated using facile processing techniques on patterned indium tin oxide coated glass substrates. The solar cells typically had a planar configuration of ITO/CH3NH3PbI3/P3HT/Ag. High sensitivity for X-rays due to high Z value, larger carrier mobility and better charge collection was observed. Detecting X-rays with energies relevant to medical oncology applications opens up the potential for diagnostic imaging applications.

Quantitative 3D comparison of biofilm imaged by X-ray micro-tomography and two-photon laser scanning microscopy.

PubMed

Larue, A E; Swider, P; Duru, P; Daviaud, D; Quintard, M; Davit, Y

2018-06-21

Optical imaging techniques for biofilm observation, like laser scanning microscopy, are not applicable when investigating biofilm formation in opaque porous media. X-ray micro-tomography (X-ray CMT) might be an alternative but it finds limitations in similarity of X-ray absorption coefficients for the biofilm and aqueous phases. To overcome this difficulty, barium sulphate was used in Davit et al. (2011) to enable high-resolution 3D imaging of biofilm via X-ray CMT. However, this approach lacks comparison with well-established imaging methods, which are known to capture the fine structures of biofilms, as well as uncertainty quantification. Here, we compare two-photon laser scanning microscopy (TPLSM) images of Pseudomonas Aeruginosa biofilm grown in glass capillaries against X-ray CMT using an improved protocol where barium sulphate is combined with low-gelling temperature agarose to avoid sedimentation. Calibrated phantoms consisting of mono-dispersed fluorescent and X-ray absorbent beads were used to evaluate the uncertainty associated with our protocol along with three different segmentation techniques, namely hysteresis, watershed and region growing, to determine the bias relative to image binarization. Metrics such as volume, 3D surface area and thickness were measured and comparison of both imaging modalities shows that X-ray CMT of biofilm using our protocol yields an accuracy that is comparable and even better in certain respects than TPLSM, even in a nonporous system that is largely favourable to TPLSM. © 2018 The Authors Journal of Microscopy © 2018 Royal Microscopical Society.

Redox chemistry of a binary transition metal oxide (AB 2 O 4 ): a study of the Cu 2+ /Cu 0 and Fe 3+ /Fe 0 interconversions observed upon lithiation in a CuFe 2 O 4 battery using X-ray absorption spectroscopy

DOE PAGES

Cama, Christina A.; Pelliccione, Christopher J.; Brady, Alexander B.; ...

2016-06-06

Copper ferrite, CuFe 2 O 4, is a promising candidate for application as a high energy electrode material in lithium based batteries. Mechanistic insight on the electrochemical reduction and oxidation processes was gained through the first X-ray absorption spectroscopic study of lithiation and delithiation of CuFe 2 O 4. A phase pure tetragonal CuFe 2 O 4 material was prepared and characterized using laboratory and synchrotron X-ray diffraction, Raman spectroscopy, and transmission electron microscopy. We used ex situ X-ray absorption spectroscopy (XAS) measurements to study the battery redox processes at the Fe and Cu K-edges, using X-ray absorption near-edge structuremore » (XANES), extended X-ray absorption fine structure (EXAFS), and transmission X-ray microscopy (TXM) spectroscopies. EXAFS analysis showed upon discharge, an initial conversion of 50% of the copper(II) to copper metal positioned outside of the spinel structure, followed by a migration of tetrahedral iron(III) cations to octahedral positions previously occupied by copper(II). Then, upon charging to 3.5 V, the copper metal remained in the metallic state, while iron metal oxidation to iron(III) was achieved. Our results provide new mechanistic insight regarding the evolution of the local coordination environments at the iron and copper centers upon discharging and charging.« less

Redox chemistry of a binary transition metal oxide (AB2O4): a study of the Cu(2+)/Cu(0) and Fe(3+)/Fe(0) interconversions observed upon lithiation in a CuFe2O4 battery using X-ray absorption spectroscopy.

PubMed

Cama, Christina A; Pelliccione, Christopher J; Brady, Alexander B; Li, Jing; Stach, Eric A; Wang, Jiajun; Wang, Jun; Takeuchi, Esther S; Takeuchi, Kenneth J; Marschilok, Amy C

2016-06-22

Copper ferrite, CuFe2O4, is a promising candidate for application as a high energy electrode material in lithium based batteries. Mechanistic insight on the electrochemical reduction and oxidation processes was gained through the first X-ray absorption spectroscopic study of lithiation and delithiation of CuFe2O4. A phase pure tetragonal CuFe2O4 material was prepared and characterized using laboratory and synchrotron X-ray diffraction, Raman spectroscopy, and transmission electron microscopy. Ex situ X-ray absorption spectroscopy (XAS) measurements were used to study the battery redox processes at the Fe and Cu K-edges, using X-ray absorption near-edge structure (XANES), extended X-ray absorption fine structure (EXAFS), and transmission X-ray microscopy (TXM) spectroscopies. EXAFS analysis showed upon discharge, an initial conversion of 50% of the copper(ii) to copper metal positioned outside of the spinel structure, followed by a migration of tetrahedral iron(iii) cations to octahedral positions previously occupied by copper(ii). Upon charging to 3.5 V, the copper metal remained in the metallic state, while iron metal oxidation to iron(iii) was achieved. The results provide new mechanistic insight regarding the evolution of the local coordination environments at the iron and copper centers upon discharging and charging.

X-ray-induced photo-chemistry and X-ray absorption spectroscopy of biological samples

PubMed Central

George, Graham N.; Pickering, Ingrid J.; Pushie, M. Jake; Nienaber, Kurt; Hackett, Mark J.; Ascone, Isabella; Hedman, Britt; Hodgson, Keith O.; Aitken, Jade B.; Levina, Aviva; Glover, Christopher; Lay, Peter A.

2012-01-01

As synchrotron light sources and optics deliver greater photon flux on samples, X-ray-induced photo-chemistry is increasingly encountered in X-ray absorption spectroscopy (XAS) experiments. The resulting problems are particularly pronounced for biological XAS experiments. This is because biological samples are very often quite dilute and therefore require signal averaging to achieve adequate signal-to-noise ratios, with correspondingly greater exposures to the X-ray beam. This paper reviews the origins of photo-reduction and photo-oxidation, the impact that they can have on active site structure, and the methods that can be used to provide relief from X-ray-induced photo-chemical artifacts. PMID:23093745

High energy x-ray phase contrast CT using glancing-angle grating interferometers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sarapata, A., E-mail: adrian.sarapata@tum.de; Stayman, J. W.; Siewerdsen, J. H.

Purpose: The authors present initial progress toward a clinically compatible x-ray phase contrast CT system, using glancing-angle x-ray grating interferometry to provide high contrast soft tissue images at estimated by computer simulation dose levels comparable to conventional absorption based CT. Methods: DPC-CT scans of a joint phantom and of soft tissues were performed in order to answer several important questions from a clinical setup point of view. A comparison between high and low fringe visibility systems is presented. The standard phase stepping method was compared with sliding window interlaced scanning. Using estimated dose values obtained with a Monte-Carlo code themore » authors studied the dependence of the phase image contrast on exposure time and dose. Results: Using a glancing angle interferometer at high x-ray energy (∼45 keV mean value) in combination with a conventional x-ray tube the authors achieved fringe visibility values of nearly 50%, never reported before. High fringe visibility is shown to be an indispensable parameter for a potential clinical scanner. Sliding window interlaced scanning proved to have higher SNRs and CNRs in a region of interest and to also be a crucial part of a low dose CT system. DPC-CT images of a soft tissue phantom at exposures in the range typical for absorption based CT of musculoskeletal extremities were obtained. Assuming a human knee as the CT target, good soft tissue phase contrast could be obtained at an estimated absorbed dose level around 8 mGy, similar to conventional CT. Conclusions: DPC-CT with glancing-angle interferometers provides improved soft tissue contrast over absorption CT even at clinically compatible dose levels (estimated by a Monte-Carlo computer simulation). Further steps in image processing, data reconstruction, and spectral matching could make the technique fully clinically compatible. Nevertheless, due to its increased scan time and complexity the technique should be thought of not as replacing, but as complimentary to conventional CT, to be used in specific applications.« less

X-ray two-photon absorption with high fluence XFEL pulses

DOE PAGES

Hoszowska, Joanna; Szlachetko, J.; Dousse, J. -Cl.; ...

2015-09-07

Here, we report on nonlinear interaction of solid Fe with intense femtosecond hard x-ray free-electron laser (XFEL) pulses. The experiment was performed at the CXI end-station of the Linac Coherent Light Source (LCLS) by means of high- resolution x-ray emission spectroscopy. The focused x-ray beam provided extreme fluence of ~10 5 photons/Å 2. Two-photon absorption leading to K-shell hollow atom formation and to single K-shell ionization of solid Fe was investigated.

BX90: A new diamond anvil cell design for X-ray diffraction and optical measurements

NASA Astrophysics Data System (ADS)

Kantor, I.; Prakapenka, V.; Kantor, A.; Dera, P.; Kurnosov, A.; Sinogeikin, S.; Dubrovinskaia, N.; Dubrovinsky, L.

2012-12-01

We present a new design of a universal diamond anvil cell, suitable for different kinds of experimental studies under high pressures. Main features of the cell are an ultimate 90-degrees symmetrical axial opening and high stability, making the presented cell design suitable for a whole range of techniques from optical absorption to single-crystal X-ray diffraction studies, also in combination with external resistive or double-side laser heating. Three examples of the cell applications are provided: a Brillouin scattering of neon, single-crystal X-ray diffraction of α-Cr2O3, and resistivity measurements on the (Mg0.60Fe0.40)(Si0.63Al0.37)O3 silicate perovskite.

Interfacial Magnetism in Complex Oxide Heterostructures Probed by Neutrons and X-rays

DOE PAGES

Liu, Yaohua; Ke, Xianglin

2015-09-02

Magnetic complex-oxide heterostructures are of keen interest because a wealth of phenomena at the interface of dissimilar materials can give rise to fundamentally new physics and potentially valuable functionalities. Altered magnetization, novel magnetic coupling and emergent interfacial magnetism at the epitaxial layered-oxide interfaces have all been intensively investigated, which shapes our understanding on how to utilize those materials, particularly for spintronics. Neutron and x-ray based techniques have played a decisive role in characterizing interfacial magnetic structures and clarifying the underlying physics in this rapidly developing field. Here we review some recent experimental results, with an emphasis on those studied viamore » polarized neutron reflectometery and polarized x-ray absorption spectroscopy. We conclude with some perspectives.« less

The magnetic order of GdMn₂Ge₂ studied by neutron diffraction and x-ray resonant magnetic scattering.

PubMed

Granovsky, S A; Kreyssig, A; Doerr, M; Ritter, C; Dudzik, E; Feyerherm, R; Canfield, P C; Loewenhaupt, M

2010-06-09

The magnetic structure of GdMn₂Ge₂ (tetragonal I4/mmm) has been studied by hot neutron powder diffraction and x-ray resonant magnetic scattering techniques. These measurements, along with the results of bulk experiments, confirm the collinear ferrimagnetic structure with moment direction parallel to the c-axis below T(C) = 96 K and the collinear antiferromagnetic phase in the temperature region T(C) < T < T(N) = 365 K. In the antiferromagnetic phase, x-ray resonant magnetic scattering has been detected at Mn K and Gd L₂ absorption edges. The Gd contribution is a result of an induced Gd 5d electron polarization caused by the antiferromagnetic order of Mn-moments.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Feng, Huan; Zhang, Weiguo; Qian, Yu

This study investigates the distributions of Br, Ca, Cl, Cr, Cu, K, Fe, Mn, Pb, Ti, V and Zn inPhragmites australisroot system and the function of Fe nanoparticles in scavenging metals in the root epidermis using synchrotron X-ray microfluorescence, synchrotron transmission X-ray microscope measurement and synchrotron X-ray absorption near-edge structure techniques. The purpose of this study is to understand the mobility of metals in wetland plant root systems after their uptake from rhizosphere soils.Phragmites australissamples were collected in the Yangtze River intertidal zone in July 2013. The results indicate that Fe nanoparticles are present in the root epidermis and thatmore » other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis.« less

Interfacial magnetism in complex oxide heterostructures probed by neutrons and x-rays.

PubMed

Liu, Yaohua; Ke, Xianglin

2015-09-23

Magnetic complex-oxide heterostructures are of keen interest because a wealth of phenomena at the interface of dissimilar materials can give rise to fundamentally new physics and potentially valuable functionalities. Altered magnetization, novel magnetic coupling and emergent interfacial magnetism at the epitaxial layered-oxide interfaces are under intensive investigation, which shapes our understanding on how to utilize those materials, particularly for spintronics. Neutron and x-ray based techniques have played a decisive role in characterizing interfacial magnetic structures and clarifying the underlying physics in this rapidly developing field. Here we review some recent experimental results, with an emphasis on those studied via polarized neutron reflectometery and polarized x-ray absorption spectroscopy. We conclude with some perspectives.

3D investigation of inclusions in diamonds using X-ray micro-tomography

NASA Astrophysics Data System (ADS)

Parisatto, M.; Nestola, F.; Artioli, G.; Nimis, P.; Harris, J. W.; Kopylova, M.; Pearson, G. D.

2012-04-01

The study of mineral inclusions in diamonds is providing invaluable insights into the geochemistry, geodynamics and geophysics of the Earth's mantle. Over the last two decades, the identification of different inclusion assemblages allowed to recognize diamonds deriving from the deep upper mantle, the transition zone and even the lower mantle. In such research field the in-situ investigation of inclusions using non-destructive techniques is often essential but still remains a challenging task. In particular, conventional 2D imaging techniques (e.g. SEM) are limited to the investigation of surfaces and the lack of access to the third dimension represents a major limitation when trying to extract quantitative information. Another critical aspect is related to sample preparation (cutting, polishing) which is typically very invasive. Nowadays, X-ray computed micro-tomography (X-μCT) allows to overcome such limitations, enabling the internal microstructure of totally undisturbed samples to be visualized in a three-dimensional (3D) manner at the sub-micrometric scale. The final output of a micro-tomography experiment is a greyvalue 3D map of the variations of the X-ray attenuation coefficient (µ) within the studied object. The high X-ray absorption contrast between diamond (almost transparent to X-rays) and the typical inclusion-forming minerals (olivines, garnets, pyroxenes, oxides and sulphides) makes X-μCT a straightforward method for the 3D visualization of inclusions and for the study of their spatial relationships with the diamond host. In this work we applied microfocus X-μCT to investigate silicate inclusions still trapped in diamonds, in order to obtain in-situ information on their exact position, crystal size, shape and X-ray absorption coefficient (which is related to their composition). We selected diamond samples from different deposits containing mainly olivine and garnet inclusions. The investigated samples derived from the Udachnaya pipe (Siberia, Russia), the Jericho Kimberlite (Slave Craton, Canada) and São Luiz-Juina (Brazil). The information obtained by tomographic experiments were combined with X-ray single-crystal diffraction data (see Nestola et al 2011) in order to identify the inclusion parageneses (peridotitic, eclogitic or websteritic) and to finally determine the origin of the studied diamonds. Our results showed that, by combining X-μCT with X-ray diffraction data, it is possible to exactly determine the 3D position of each inclusion together with their crystal size, even though they cannot be detected by using an optical microscope. In addition, such method could have strong crystallographic implications for inclusions still trapped in diamonds as it enables the application of a reliable numerical absorption correction to the 3D intensity data collections. REF. Nestola, F., Nimis, P., Ziberna, L., Longo, M., Marzoli, A., Harris, J.W., Manghnani, M.H., Fedortchouk, Y. (2011): First crystal-structure determination of olivine in diamond: composition and implications for provenance in the Earth's mantle. Earth Planet. Sci. Lett., 305, 249-255.

A low cost method for hard x-ray grating interferometry.

PubMed

Du, Yang; Lei, Yaohu; Liu, Xin; Huang, Jianheng; Zhao, Zhigang; Guo, Jinchuan; Li, Ji; Niu, Hanben

2016-12-07

Grating interferometry is advantageous over conventional x-ray absorption imaging because it enables the detection of samples constituted by low atomic number elements (low-Z materials). Therefore, it has a potential application in biological science and medical diagnostics. The grating interferometry has some critical optics components such as absorption gratings which are conventionally manufactured by the lithography, electroplating, and molding (LIGA) technique and employing gold as the absorbent material in it. However, great challenge lies in its implementations for practical applications because of the cost and difficulty to achieve high aspect ratio absorbing grating devices. In this paper, we present a low-cost approach that involves using the micro-casting technique with bismuth (Bi) as the absorber in source grating and as well as filling cesium iodide thallium(CsI:Tl) in a periodically structured scintillator. No costly facilities as synchrotron radiation are required and cheap material is used in our approach. Our experiment using these components shows high quality complementary images can be obtained with contrast of absorption, phase and visibility. This alternative method conquers the limitation of costly grating devices for a long time and stands an important step towards the further practical application of grating interferometry.

Hard x-ray phase contrastmicroscopy - techniques and applications

NASA Astrophysics Data System (ADS)

Holzner, Christian

In 1918, Einstein provided the first description of the nature of the refractive index for X-rays, showing that phase contrast effects are significant. A century later, most x-ray microscopy and nearly all medical imaging remains based on absorption contrast, even though phase contrast offers orders of magnitude improvements in contrast and reduced radiation exposure at multi-keV x-ray energies. The work presented is concerned with developing practical and quantitative methods of phase contrast for x-ray microscopy. A theoretical framework for imaging in phase contrast is put forward; this is used to obtain quantitative images in a scanning microscope using a segmented detector, and to correct for artifacts in a commercial phase contrast x-ray nano-tomography system. The principle of reciprocity between scanning and full-field microscopes is then used to arrive at a novel solution: Zernike contrast in a scanning microscope. These approaches are compared on a theoretical and experimental basis in direct connection with applications using multi-keV x-ray microscopes at the Advanced Photon Source at Argonne National Laboratory. Phase contrast provides the best means to image mass and ultrastructure of light elements that mainly constitute biological matter, while stimulated x-ray fluorescence provides high sensitivity for studies of the distribution of heavier trace elements, such as metals. These approaches are combined in a complementary way to yield quantitative maps of elemental concentration from 2D images, with elements placed in their ultrastructural context. The combination of x-ray fluorescence and phase contrast poses an ideal match for routine, high resolution tomographic imaging of biological samples in the future. The presented techniques and demonstration experiments will help pave the way for this development.

Correction of absorption-edge artifacts in polychromatic X-ray tomography in a scanning electron microscope for 3D microelectronics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Laloum, D., E-mail: david.laloum@cea.fr; CEA, LETI, MINATEC Campus, 17 rue des Martyrs, 38054 Grenoble Cedex 9; STMicroelectronics, 850 rue Jean Monnet, 38926 Crolles

2015-01-15

X-ray tomography is widely used in materials science. However, X-ray scanners are often based on polychromatic radiation that creates artifacts such as dark streaks. We show this artifact is not always due to beam hardening. It may appear when scanning samples with high-Z elements inside a low-Z matrix because of the high-Z element absorption edge: X-rays whose energy is above this edge are strongly absorbed, violating the exponential decay assumption for reconstruction algorithms and generating dark streaks. A method is proposed to limit the absorption edge effect and is applied on a microelectronic case to suppress dark streaks between interconnections.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mukerjee, S.; Ziegelbauer, J; Arruda, T

Over the last few decades, researchers have made significant developments in producing more advanced electrocatalytic materials for power generation applications. For example, traditional fuel cell catalysts often involve high-priced precious metals such as Pt. However, in order for fuel cells to become commercially viable, there is a need to reduce or completely remove precious metal altogether. As a result, a myriad of novel, unconventional materials have been explored such as chalcogenides, porphyrins, and organic-metal-macrocycles for low/medium temperature fuel cells as well as enzymatic and microbial fuel cells. As these materials increasingly become more complex, researchers often find themselves in searchmore » of new characterization methods, especially those which are allow in situ and operando measurements with element specificity. One such method that has received much attention for analysis of electrocatalytic materials is X-ray absorption spectroscopy (XAS). XAS is an element specific, core level absorption technique which yields structural and electronic information. As a core electron method, XAS requires an extremely bright source, hence a synchrotron. The resulting intensity of synchrotron radiation allow for experiments to be conducted in situ, under electrochemically relevant conditions. Although a bulk-averaging technique requiring rigorous mathematical manipulation, XAS has the added benefit that it can probe materials which possess no long range order. This makes it ideal to characterize nano-scale electrocatalysts. XAS experiments are conducted by ramping the X-ray photon energy while measuring absorption of the incident beam the sample or by counting fluorescent photons released from a sample due to subsequent relaxation. Absorption mode XAS follows the Beer-Lambert Law, {mu}x = log(I{sub 0}/I{sub t}) (1) where {mu} is the absorption coefficient, x is the sample thickness and I{sub 0} and I{sub t} are the intensities of the incident and transmission beams respectively. When the energy of the incident X-rays exceed the electron binding energy (E{sub 0}) of the element under investigation, the electron is ejected from the core to available excited states in the form of a photoelectron with kinetic energy: E{sub k} = h? - E{sub 0} (2) with, E{sub k} being the kinetic energy of the released photoelectron and h? the energy of the incident beam. In general, the X-ray absorption spectrum is broken down into two distinct energy regions: the X-ray absorption near-edge structure or XANES (-50eV {le} E{sub 0} {le} 50eV) and the extended X-ray absorption fine-structure or EXAFS (50eV {le} E{sub 0} {le} {approx}1000eV). The XANES region is dominated by low-energy photoelectrons which undergo multiple scattering events. As such, it can reveal information about oxidation state, local symmetry, electronic structure, and the extent of oxidation of a material. Due to this complex multiple scattering, there is no simple XANES equation to describe it quantitatively. However, recent advancements in computers and the evolution of numerical methods such as the FEFF code have made possible reliable XANES simulations. Photoelectrons in the EXAFS region have high enough E{sub k} to undergo primarily single back-scattering events. These back-scattered photoelectrons interfere with the outgoing photoelectrons, causing the oscillations in the absorption spectrum. Using the previously developed EXAFS equations it is now possible to model EXAFS data to determine coordination numbers, bond distances, and mean-square disorder (commonly referred to as Debye-Waller factor). EXAFS data is often shown by Fourier Transforming KSpace into distance, r, space where the total magnitude is plotted against the radial coordinates. This allow for easy qualitative comparison of samples. Employing EXAFS on nanoscale materials has the added advantage that it can quantitatively illustrate changes in atom-atom coordination, which can be related to particle size or morphology. Overall this technique enables the measurement of both bulk and surface adsorbed species with element specificity under actual electrochemical operating conditions. Thus this represents the one of the most powerful methods to understand the exact role of the reaction center and degradation processes such as sintering and corrosion.« less

Enhancement of X-ray dose absorption for medical applications

NASA Astrophysics Data System (ADS)

Lim, Sara; Nahar, S.; Pradhan, A.; Barth, R.

2013-05-01

A promising technique for cancer treatment is radiation therapy with high-Z (HZ) nanomoities acting as radio-sensitizers attached to tumor cells and irradiated with X-rays. But the efficacy of radiosenstization is highly energy dependent. We study the physical effects in using platinum (Pt) as the radio-sensitizing agent, coupled with commonly employed broadband x-ray sources with mean energies around 100 keV, as opposed to MeV energies produced by clinical linear accelerators (LINAC) used in radiation therapy. Numerical calculations, in vitro, and in vivo studies of F98 rat glioma (brain cancer) demonstrate that irradiation from a medium energy X-ray (MEX) 160 kV source is far more effective than from a high energy x-ray (HEX) 6 MV LINAC. We define a parameter to quantify photoionization by an x-ray source, which thereby provides a measure of subsequent Auger decays. The platinum (Z = 78) results are also relevant to ongoing studies on x-ray interaction with gold (Z = 79) nanoparticles, widely studied as an HZ contrast agent. The present study should be of additional interest for a combined radiation plus chemotherapy treatment since Pt compounds such cis-Pt and carbo-Pt are commonly used in chemotherapy.

Synchrotron X-ray microfluorescence measurement of metal distributions in Phragmites australis root system in the Yangtze River intertidal zone

DOE PAGES

Feng, Huan; Zhang, Weiguo; Qian, Yu; ...

2016-06-15

This paper investigates the distributions of Br, Ca, Cl, Cr, Cu, K, Fe, Mn, Pb, Ti, V and Zn in Phragmites australis root system and the function of Fe nanoparticles in scavenging metals in the root epidermis using synchrotron X-ray microfluorescence, synchrotron transmission X-ray microscope measurement and synchrotron X-ray absorption near-edge structure techniques. The purpose of this study is to understand the mobility of metals in wetland plant root systems after their uptake from rhizosphere soils. Phragmites australis samples were collected in the Yangtze River intertidal zone in July 2013. The results indicate that Fe nanoparticles are present in themore » root epidermis and that other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis.« less

Synchrotron X-ray microfluorescence measurement of metal distributions in Phragmites australis root system in the Yangtze River intertidal zone

DOE Office of Scientific and Technical Information (OSTI.GOV)

Feng, Huan; Zhang, Weiguo; Qian, Yu

This paper investigates the distributions of Br, Ca, Cl, Cr, Cu, K, Fe, Mn, Pb, Ti, V and Zn in Phragmites australis root system and the function of Fe nanoparticles in scavenging metals in the root epidermis using synchrotron X-ray microfluorescence, synchrotron transmission X-ray microscope measurement and synchrotron X-ray absorption near-edge structure techniques. The purpose of this study is to understand the mobility of metals in wetland plant root systems after their uptake from rhizosphere soils. Phragmites australis samples were collected in the Yangtze River intertidal zone in July 2013. The results indicate that Fe nanoparticles are present in themore » root epidermis and that other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis.« less

Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II

DOE PAGES

Nazaretski, E.; Yan, H.; Lauer, K.; ...

2017-10-05

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ~15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature ofmore » a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.« less

Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nazaretski, E.; Yan, H.; Lauer, K.

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ~15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature ofmore » a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.« less

Creation of X-Ray Transparency of Matter by Stimulated Elastic Forward Scattering.

PubMed

Stöhr, J; Scherz, A

2015-09-04

X-ray absorption by matter has long been described by the famous Beer-Lambert law. Here, we show how this fundamental law needs to be modified for high-intensity coherent x-ray pulses, now available at x-ray free electron lasers, due to the onset of stimulated elastic forward scattering. We present an analytical expression for the modified polarization-dependent Beer-Lambert law for the case of resonant core-to-valence electronic transitions and incident transform limited x-ray pulses. Upon transmission through a solid, the resonant absorption and dichroic contrasts are found to vanish with increasing x-ray intensity, with the stimulation threshold lowered by orders of magnitude through a resonant superradiantlike effect. Our results have broad implications for the study of matter with x-ray lasers.

Creation of X-Ray Transparency of Matter by Stimulated Elastic Forward Scattering

NASA Astrophysics Data System (ADS)

Stöhr, J.; Scherz, A.

2015-09-01

X-ray absorption by matter has long been described by the famous Beer-Lambert law. Here, we show how this fundamental law needs to be modified for high-intensity coherent x-ray pulses, now available at x-ray free electron lasers, due to the onset of stimulated elastic forward scattering. We present an analytical expression for the modified polarization-dependent Beer-Lambert law for the case of resonant core-to-valence electronic transitions and incident transform limited x-ray pulses. Upon transmission through a solid, the resonant absorption and dichroic contrasts are found to vanish with increasing x-ray intensity, with the stimulation threshold lowered by orders of magnitude through a resonant superradiantlike effect. Our results have broad implications for the study of matter with x-ray lasers.

Flash x-ray radiography of argon jets in ambient air

NASA Astrophysics Data System (ADS)

Geiswiller, J.; Robert, E.; Huré, L.; Cachoncinlle, C.; Viladrosa, R.; Pouvesle, J. M.

1998-09-01

This paper describes the development and application of a soft x-ray flash radiography technique. A very compact soft x-ray flash source has been specially designed for these studies. The table-top x-ray source developed in this work emits strong doses, up to one roentgen at the output window, of x-ray photons, with most of them in the characteristic lines of the anode material (photon energy in the energy range 5-10 keV), in pulse of 20 ns FWHM with an x-ray emission zone smaller than 0957-0233/9/9/024/img1. All these characteristics make this source attractive for the x-ray radiography of high-speed phenomena, down to ten nanoseconds duration and/or for the media presenting weak absorption for the harder x-ray photons emitted by more conventional flash x-ray systems. Argon streams in ambient air were chosen as a typical case to enlighten the potentialities of this method. Single-shot radiographs of such an argon jet through rectangular nozzles were obtained. No attempt of quantitative measurement of local density in the argon stream has yet been performed, only the qualitative structure of the jet has been investigated. Nevertheless, these preliminary results enable us to state that the diagnostics of gaseous or plasma media, even at rather low pressures, can proceed using soft x-ray flash radiography.

High Redshift Quasars

NASA Technical Reports Server (NTRS)

Elvis, Martin S.

1996-01-01

The report for this period includes three papers: 'Associated Absorption at Low and High Redshift'; 'Strong X-ray Absorption in a Broad Absorption Line Quasar: PHL5200'; and 'ASCA and ROSAT X-ray Spectra of High-Redshift Radio-Loud Quasars'. The first gives examples from both low and high redshift for combining information on absorbing material in active galactic nuclei from both x-ray and the UV. The second presents ASCA observations of the z = 1.98 prototype broad absorption line quasar (BALQSO): PHL 5200, detected with both the solid-state imaging spectrometers and the gas imaging spectometers. The third paper presents results on the x-ray properties of 9 high-redshift radio-loud quasars observed by ASCA and ROSAT, including ASCA observations of S5 0014+81 (z = 3.38) and S5 0836+71 (z = 2.17) and ROSAT observations of PKS 2126-158.

CHANDRA Detects Relativistic Broad Absorption Lines from APM 08279+5255

NASA Astrophysics Data System (ADS)

Chartas, G.; Brandt, W. N.; Gallagher, S. C.; Garmire, G. P.

2002-11-01

We report the discovery of X-ray broad absorption lines (BALs) from the BAL quasar APM 08279+5255 originating from material moving at relativistic velocities with respect to the central source. The large flux magnification by a factor of ~100 provided by the gravitational lens effect combined with the large redshift (z=3.91) of the quasar have facilitated the acquisition of the first high signal-to-noise X-ray spectrum of a quasar containing X-ray BALs. Our analysis of the X-ray spectrum of APM 08279+5255 places the rest-frame energies of the two observed absorption lines at 8.1 and 9.8 keV. The detection of each of these lines is significant at a greater than 99.9% confidence level based on the F-test. Assuming that the absorption lines are from Fe XXV Kα, the implied bulk velocities of the X-ray BALs are ~0.2c and ~0.4c, respectively. The observed high bulk velocities of the X-ray BALs combined with the relatively short recombination timescales of the X-ray-absorbing gas imply that the absorbers responsible for the X-ray BALs are located at radii of <~2×1017 cm, within the expected location of the UV absorber. With this implied geometry, the X-ray gas could provide the necessary shielding to prevent the UV absorber from being completely ionized by the central X-ray source, consistent with hydrodynamical simulations of line-driven disk winds. Estimated mass-outflow rates for the gas creating the X-ray BALs are typically less than a solar mass per year. Our spectral analysis also indicates that the continuum X-ray emission of APM 08279+5255 is consistent with that of a typical radio-quiet quasar with a spectral slope of Γ=1.72+0.06-0.05.

Hybrid modelling of a high-power X-ray attenuator plasma.

PubMed

Martín Ortega, Álvaro; Lacoste, Ana; Minea, Tiberiu

2018-05-01

X-ray gas attenuators act as stress-free high-pass filters for synchrotron and free-electron laser beamlines to reduce the heat load in downstream optical elements without affecting other properties of the X-ray beam. The absorption of the X-ray beam triggers a cascade of processes that ionize and heat up the gas locally, changing its density and therefore the X-ray absorption. Aiming to understand and predict the behaviour of the gas attenuator in terms of efficiency versus gas pressure, a hybrid model has been developed, combining three approaches: an analytical description of the X-ray absorption; Monte Carlo for the electron thermalization; and a fluid treatment for the electron diffusion, recombination and excited-states relaxation. The model was applied to an argon-filled attenuator prototype built and tested at the European Synchrotron Radiation Facility, at a pressure of 200 mbar and assuming stationary conditions. The results of the model showed that the electron population thermalizes within a few nanoseconds after the X-ray pulse arrival and it occurs just around the X-ray beam path, recombining in the bulk of the gas rather than diffusing to the attenuator walls. The gas temperature along the beam path reached 850 K for 770 W of incident power and 182 W m -1 of absorbed power. Around 70% of the absorbed power is released as visible and UV radiation rather than as heat to the gas. Comparison of the power absorption with the experiment showed an overall agreement both with the plasma radial profile and power absorption trend, the latter within an error smaller than 20%. This model can be used for the design and operation of synchrotron gas attenuators and as a base for a time-dependent model for free-electron laser attenuators.

X-Ray Absorption Spectroscopy As a Probe of Microbial Sulfur Biochemistry: the Nature of Bacterial Sulfur Globules Revisited

DOE Office of Scientific and Technical Information (OSTI.GOV)

George, G.N.; Gnida, M.; Bazylinski, D.A.

2009-05-18

The chemical nature of the sulfur in bacterial sulfur globules has been the subject of controversy for a number of years. Sulfur K-edge X-ray absorption spectroscopy (XAS) is a powerful technique for probing the chemical forms of sulfur in situ, but two groups have used it with very different conclusions. The root of the controversy lies with the different detection strategies used by the two groups, which result in very different spectra. This paper seeks to resolve the controversy. We experimentally demonstrate that the use of transmittance detection for sulfur K-edge XAS measurements is highly prone to spectroscopic distortions andmore » that much of the published work on sulfur bacteria is very likely based on distorted data. We also demonstrate that all three detection methods used for X-ray absorption experiments yield essentially identical spectra when the measurements are carried out under conditions where no experimental distortions are expected. Finally, we turn to the original question--the chemical nature of bacterial sulfur. We examine isolated sulfur globules of Allochromatium vinosum and intact cells of a strain of magnetotactic coccus and show that XAS indicates the presence of a chemical form of sulfur resembling S{sub 8}.« less

EUV spectroscopy of high-redshift x-ray objects

NASA Astrophysics Data System (ADS)

Kowalski, M. P.; Wolff, M. T.; Wood, K. S.; Barbee, T. W., Jr.; Barstow, M. A.

2010-07-01

As astronomical observations are pushed to cosmological distances (z>3) the spectral energy distributions of X-ray objects, AGN for example, will be redshifted into the EUV waveband. Consequently, a wealth of critical spectral diagnostics, provided by, for example, the Fe L-shell complex and the O VII/VIII lines, will be lost to future planned X-ray missions (e.g., IXO, Gen-X) if operated at traditional X-ray energies. This opens up a critical gap in performance located at short EUV wavelengths, where critical X-ray spectral transitions occur in high-z objects. However, normal-incidence multilayer-grating technology, which performs best precisely at such wavelengths, together with advanced nanolaminate replication techniques have been developed and are now mature to the point where advanced EUV instrument designs with performance complementary to IXO and Gen-X are practical. Such EUV instruments could be flown either independently or as secondary instruments on these X-ray missions. We present here a critical examination of the limits placed on extragalactic EUV measurements by ISM absorption, the range where high-z measurements are practical, and the requirements this imposes on next-generation instrument designs. We conclude with a discussion of a breakthrough technology, nanolaminate replication, which enables such instruments.

X-Ray Studies of Diffusion Dynamics in Nano-Confined Geometries

NASA Astrophysics Data System (ADS)

Boucheron, Leandra

Since their discovery in the late 1800s, x-rays have taken the stage as one of the most powerful research techniques for materials science. Their element-specific absorption has allowed for everyday applications in security and medical imaging, while their short wavelength has a tremendous ability to resolve materials on a molecular or even atomic level. In this dissertation, I will discuss basic properties of x-rays as well as how they are produced and detected. I will also present x-ray scattering and analysis techniques before moving onto a discussion of my research on diffusion in soft-matter systems. I provide a full alignment guide for a lab-based dynamic light scattering (DLS) goniometer system, which I used for some preliminary studies of systems. I proceed to discuss diffusion on the nanoscale in quasi-1D (nanopores) and quasi-2D (liquid surface) systems. The latter of these systems was the main focus of my dissertation research. I utilized x-ray photon correlation spectroscopy (XPCS) to study the diffusion and interparticle dynamics of iron oxide nanoparticles at the air-water interface. Autocorrelation analysis revealed that these particles show signatures of a jammed system under lateral compression. I present these results as well as a description of their interpretation and importance in the main text.

Insights on the X-ray weak quasar phenomenon from XMM-Newton monitoring of PHL 1092

NASA Astrophysics Data System (ADS)

Miniutti, G.; Brandt, W. N.; Schneider, D. P.; Fabian, A. C.; Gallo, L. C.; Boller, Th.

2012-09-01

PHL 1092 is a z ˜ 0.4 high-luminosity counterpart of the class of Narrow-Line Seyfert 1 galaxies. In 2008, PHL 1092 was found to be in a remarkably low X-ray flux state during an XMM-Newton observation. Its 2 keV flux density had dropped by a factor of ˜260 with respect to a previous observation performed 4.5 yr earlier. The ultraviolet (UV) flux remained almost constant, resulting in a significant steepening of the optical-to-X-ray slope αox from -1.57 to -2.51, making PHL 1092 one of the most extreme X-ray weak quasars with no observed broad absorption lines (BALs) in the UV. We have monitored the source since 2008 with three further XMM-Newton observations, producing a simultaneous UV and X-ray data base spanning almost 10 yr in total in the activity of the source. Our monitoring programme demonstrates that the αox variability in PHL 1092 is entirely driven by long-term X-ray flux changes. We apply a series of physically motivated models with the goal of explaining the UV-to-X-ray spectral energy distribution and the extreme X-ray and αox variability. We consider three possible models. (i) A breathing corona scenario in which the size of the X-ray-emitting corona is correlated with the X-ray flux. In this case, the lowest X-ray flux states of PHL 1092 are associated with an almost complete collapse of the X-ray corona down to the marginal stable orbit. (ii) An absorption scenario in which the X-ray flux variability is entirely due to intervening absorption. If so, PHL 1092 is a quasar with standard X-ray output for its optical luminosity, appearing as X-ray weak at times due to absorption. (iii) A disc-reflection-dominated scenario in which the X-ray-emitting corona is confined within a few gravitational radii from the black hole at all times. In this case, the intrinsic variability of PHL 1092 only needs to be a factor of ˜10 rather than the observed factor of ˜260. We discuss these scenarios in the context of non-BAL X-ray weak quasars.

Controlled surface segregation leads to efficient coke-resistant nickel/platinum bimetallic catalysts for the dry reforming of methane

DOE PAGES

Li, Lidong; Zhou, Lu; Ould-Chikh, Samy; ...

2015-02-03

Surface composition and structure are of vital importance for heterogeneous catalysts, especially for bimetallic catalysts, which often vary as a function of reaction conditions (known as surface segregation). The preparation of bimetallic catalysts with controlled metal surface composition and structure is very challenging. In this study, we synthesize a series of Ni/Pt bimetallic catalysts with controlled metal surface composition and structure using a method derived from surface organometallic chemistry. The evolution of the surface composition and structure of the obtained bimetallic catalysts under simulated reaction conditions is investigated by various techniques, which include CO-probe IR spectroscopy, high-angle annular dark-field scanningmore » transmission electron microscopy, energy-dispersive X-ray spectroscopy, extended X-ray absorption fine structure analysis, X-ray absorption near-edge structure analysis, XRD, and X-ray photoelectron spectroscopy. It is demonstrated that the structure of the bimetallic catalyst is evolved from Pt monolayer island-modified Ni nanoparticles to core–shell bimetallic nanoparticles composed of a Ni-rich core and a Ni/Pt alloy shell upon thermal treatment. As a result, these catalysts are active for the dry reforming of methane, and their catalytic activities, stabilities, and carbon formation vary with their surface composition and structure.« less

High-throughput, high-resolution X-ray phase contrast tomographic microscopy for visualisation of soft tissue

NASA Astrophysics Data System (ADS)

McDonald, S. A.; Marone, F.; Hintermüller, C.; Bensadoun, J.-C.; Aebischer, P.; Stampanoni, M.

2009-09-01

The use of conventional absorption based X-ray microtomography can become limited for samples showing only very weak absorption contrast. However, a wide range of samples studied in biology and materials science can produce significant phase shifts of the X-ray beam, and thus the use of the phase signal can provide substantially increased contrast and therefore new and otherwise inaccessible information. The application of two approaches for high-throughput, high-resolution X-ray phase contrast tomography, both available on the TOMCAT beamline of the SLS, is illustrated. Differential Phase Contrast (DPC) imaging uses a grating interferometer and a phase-stepping technique. It has been integrated into the beamline environment on TOMCAT in terms of the fast acquisition and reconstruction of data and the availability to scan samples within an aqueous environment. The second phase contrast approach is a modified transfer of intensity approach that can yield the 3D distribution of the phase (refractive index) of a weakly absorbing object from a single tomographic dataset. These methods are being used for the evaluation of cell integrity in 3D, with the specific aim of following and analyzing progressive cell degeneration to increase knowledge of the mechanistic events of neurodegenerative disorders such as Parkinson's disease.

Local surrounding of Mn in LaMn 1-xCo xO 3 compounds by means of EXAFS on Mn-K

NASA Astrophysics Data System (ADS)

Procházka, Vít; Sikora, Marcin; Kapusta, Czeslaw; Štěpánková, Helena; Chlan, Vojtěch; Knížek, Karel; Jirák, Zdeněk

2010-05-01

A systematic study of LaMn 1-xCo xO 3 perovskite series by means of X-ray absorption spectroscopy in the extended X-ray absorption fine structure (EXAFS) range of the K-absorption edge of Mn is reported. The Mn-K edge absorption measurements in the EXAFS region were performed to study the local surrounding of Mn ions. Polycrystalline powder samples of LaMn 1-xCo xO 3 ( x=0, 0.02; 0.2; 0.4; 0.5; 0.6; 0.8) prepared by solid-state reaction were used. The EXAFS spectra were analyzed with the FEFF8 computer program. The Mn-O distances of Mn to the nearest oxygen surroundings were evaluated for the samples in the series and compared with the Co-O distances obtained by EXAFS in V. Procházka et al., JMMM 310 (2007) 197 and with results of X-ray powder diffraction in C. Autret, J. Phys. Condens. Matter 17 (2005) 1601.

Geoscience Applications of Synchrotron X-ray Computed Microtomography

NASA Astrophysics Data System (ADS)

Rivers, M. L.

2009-05-01

Computed microtomography is the extension to micron spatial resolution of the CAT scanning technique developed for medical imaging. Synchrotron sources are ideal for the method, since they provide a monochromatic, parallel beam with high intensity. High energy storage rings such as the Advanced Photon Source at Argonne National Laboratory produce x-rays with high energy, high brilliance, and high coherence. All of these factors combine to produce an extremely powerful imaging tool for earth science research. Techniques that have been developed include: - Absorption and phase contrast computed tomography with spatial resolution approaching one micron - Differential contrast computed tomography, imaging above and below the absorption edge of a particular element - High-pressure tomography, imaging inside a pressure cell at pressures above 10GPa - High speed radiography, with 100 microsecond temporal resolution - Fluorescence tomography, imaging the 3-D distribution of elements present at ppm concentrations. - Radiographic strain measurements during deformation at high confining pressure, combined with precise x- ray diffraction measurements to determine stress. These techniques have been applied to important problems in earth and environmental sciences, including: - The 3-D distribution of aqueous and organic liquids in porous media, with applications in contaminated groundwater and petroleum recovery. - The kinetics of bubble formation in magma chambers, which control explosive volcanism. - Accurate crystal size distributions in volcanic systems, important for understanding the evolution of magma chambers. - The equation-of-state of amorphous materials at high pressure using both direct measurements of volume as a function of pressure and also by measuring the change x-ray absorption coefficient as a function of pressure. - The formation of frost flowers on Arctic sea-ice, which is important in controlling the atmospheric chemistry of mercury. - The distribution of cracks in rocks at potential nuclear waste repositories. - The location and chemical speciation of toxic elements such as arsenic and nickel in soils and in plant tissues in contaminated Superfund sites. - The strength of earth materials under the pressure and temperature conditions of the Earth's mantle, providing insights into plate tectonics and the generation of earthquakes.

Structure determination from XAFS using high-accuracy measurements of x-ray mass attenuation coefficients of silver, 11 keV-28 keV, and development of an all-energies approach to local dynamical analysis of bond length, revealing variation of effective thermal contributions across the XAFS spectrum.

PubMed

Tantau, L J; Chantler, C T; Bourke, J D; Islam, M T; Payne, A T; Rae, N A; Tran, C Q

2015-07-08

We use the x-ray extended range technique (XERT) to experimentally determine the mass attenuation coefficient of silver in the x-ray energy range 11 kev-28 kev including the silver K absorption edge. The results are accurate to better than 0.1%, permitting critical tests of atomic and solid state theory. This is one of the most accurate demonstrations of cross-platform accuracy in synchrotron studies thus far. We derive the mass absorption coefficients and the imaginary component of the form factor over this range. We apply conventional XAFS analytic techniques, extended to include error propagation and uncertainty, yielding bond lengths accurate to approximately 0.24% and thermal Debye-Waller parameters accurate to 30%. We then introduce the FDMX technique for accurate analysis of such data across the full XAFS spectrum, built on full-potential theory, yielding a bond length accuracy of order 0.1% and the demonstration that a single Debye parameter is inadequate and inconsistent across the XAFS range. Two effective Debye-Waller parameters are determined: a high-energy value based on the highly-correlated motion of bonded atoms (σ(DW) = 0.1413(21) Å), and an uncorrelated bulk value (σ(DW) = 0.1766(9) Å) in good agreement with that derived from (room-temperature) crystallography.

Shining X-rays on catalysts at work

NASA Astrophysics Data System (ADS)

Grunwaldt, J.-D.

2009-11-01

Structure-performance relationships gained by studying catalysts at work are considered the key to further development of catalysts underlined here by a brief overview on our research in this area. The partial oxidation of methane to hydrogen and carbon monoxide over Pt- and Rh-based catalysts and the total combustion of hydrocarbons demonstrate the importance of structural identification of catalysts in its working state and the measurement of the catalytic performance at the same time. Moreover, proper cell design is a key both here and in liquid phase reactions including preparation or high pressure reactions. In several cases structural changes during preparation, activation and reaction occur on a subminute scale or the catalyst structure varies inside a reactor as a result of temperature or concentration gradients. This, additionally, requires time and spatial resolution. Examples from time-resolved QEXAFS studies during the partial oxidation of methane over Pt- and Rh-based catalysts demonstrate some of the recent developments of the technique (use not only of Si(111) but also Si(311) crystals, angular encoder, full EXAFS spectra at subsecond recording time, and modulation excitation spectroscopy). In order to obtain spectroscopic information on the oxidation state inside a microreactor, scanning and full field X-ray microscopy with X-ray absorption spectroscopic contrast were achieved under reaction conditions. If a microbeam is applied, fast scanning techniques like QEXAFS are required. In this way, even X-ray absorption spectroscopic tomographic images of a slice of a microreactor were obtained. The studies were recently extended to spatiotemporal studies that give important insight into the dynamics of the catalyst structure in a spatial manner with subsecond time-resolution.

Amorphous boron gasket in diamond anvil cell research

NASA Astrophysics Data System (ADS)

Lin, Jung-Fu; Shu, Jinfu; Mao, Ho-kwang; Hemley, Russell J.; Shen, Guoyin

2003-11-01

Recent advances in high-pressure diamond anvil cell experiments include high-energy synchrotron x-ray techniques as well as new cell designs and gasketing procedures. The success of high-pressure experiments usually depends on a well-prepared sample, in which the gasket plays an important role. Various gasket materials such as diamond, beryllium, rhenium, and stainless steel have been used. Here we introduce amorphous boron as another gasket material in high-pressure diamond anvil cell experiments. We have applied the boron gasket for laser-heating x-ray diffraction, radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, and inelastic x-ray scattering. The high shear strength of the amorphous boron maximizes the thickness of the sample chamber and increases the pressure homogeneity, improving the quality of high-pressure data. Use of amorphous boron avoids unwanted x-ray diffraction peaks and reduces the absorption of incident and x rays exiting the gasket material. The high quality of the diffraction patterns makes it possible to refine the cell parameters with powder x-ray diffraction data under high pressure and high temperature. The reactivity of boron prevents its use at high temperatures, however. When heated, boron may also react with the specimen to produce unwanted phases. The relatively porous boron starting material at ambient conditions also poses some challenges for sample preparation.

An IAEA multi-technique X-ray spectrometry endstation at Elettra Sincrotrone Trieste: benchmarking results and interdisciplinary applications.

PubMed

Karydas, Andreas Germanos; Czyzycki, Mateusz; Leani, Juan José; Migliori, Alessandro; Osan, Janos; Bogovac, Mladen; Wrobel, Pawel; Vakula, Nikita; Padilla-Alvarez, Roman; Menk, Ralf Hendrik; Gol, Maryam Ghahremani; Antonelli, Matias; Tiwari, Manoj K; Caliri, Claudia; Vogel-Mikuš, Katarina; Darby, Iain; Kaiser, Ralf Bernd

2018-01-01

The International Atomic Energy Agency (IAEA) jointly with the Elettra Sincrotrone Trieste (EST) operates a multipurpose X-ray spectrometry endstation at the X-ray Fluorescence beamline (10.1L). The facility has been available to external users since the beginning of 2015 through the peer-review process of EST. Using this collaboration framework, the IAEA supports and promotes synchrotron-radiation-based research and training activities for various research groups from the IAEA Member States, especially those who have limited previous experience and resources to access a synchrotron radiation facility. This paper aims to provide a broad overview about various analytical capabilities, intrinsic features and performance figures of the IAEA X-ray spectrometry endstation through the measured results. The IAEA-EST endstation works with monochromatic X-rays in the energy range 3.7-14 keV for the Elettra storage ring operating at 2.0 or 2.4 GeV electron energy. It offers a combination of different advanced analytical probes, e.g. X-ray reflectivity, X-ray absorption fine-structure measurements, grazing-incidence X-ray fluorescence measurements, using different excitation and detection geometries, and thereby supports a comprehensive characterization for different kinds of nanostructured and bulk materials.

Theoretical studies on the structural and spectra properties of two C74 fullerenes and the chlorinated species C74Cl10

NASA Astrophysics Data System (ADS)

Zheng, Mei; Song, Xitong; Li, Xiaoqi; Qi, Jiayuan

2018-07-01

The geometrical/electronic structures, X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine structure spectroscopy of two especially C74 fullerenes (D3h-C74 and C1-C74) and the chlorinated species C1-C74Cl10, which are newly isolated in the experiment, have been calculated by means of the density functional theory (DFT) method. Effective changes in the electronic structure and simulated X-ray spectra have been observed after chlorination. Strong isomer dependence has been found in both spectra, thus the 'fingerprints' in the spectra can be employed as a tool to identify the isomers. The ultraviolet-visible (UV-vis) absorption spectrum of C1-C74Cl10 has been performed by using the time-dependent DFT method. The generated UV-vis spectrum coincides with the previous experimental counterpart. The results of this work can provide useful information especially for isomer identification and further study on fullerenes by means of the aforementioned spectroscopy techniques.

Two-Photon Absorption of Soft X-Ray Free Electron Laser Radiation by Graphite Near the Carbon K-Absorption Edge

DOE Office of Scientific and Technical Information (OSTI.GOV)

Christensen, Steven T; Lam, Royce K.; Raj, Sumana L.

We have examined the transmission of soft X-ray pulses from the FERMI free electron laser through carbon films of varying thickness, quantifying nonlinear effects of pulses above and below the carbon K-edge. At typical of soft X-ray free electron laser intensities, pulses exhibit linear absorption at photon energies above and below the K-edge, ~308 and ~260 eV, respectively; whereas two-photon absorption becomes significant slightly below the K-edge, ~284.2 eV. The measured two-photon absorption cross section at 284.18 eV (~6 x 10-48 cm4 s) is 7 orders of magnitude above what is expected from a simple theory based on hydrogen-like atomsmore » - a result of resonance effects.« less

Imaging efficiency of an X-ray contrast agent-incorporated polymeric microparticle.

PubMed

Ahn, Sungsook; Jung, Sung Yong; Lee, Jin Pyung; Lee, Sang Joon

2011-01-01

Biocompatible polymeric encapsulants have been widely used as a delivery vehicle for a variety of drugs and imaging agents. In this study, X-ray contrast agent (iopamidol) is encapsulated into a polymeric microparticle (polyvinyl alcohol) as a particulate flow tracer in synchrotron X-ray imaging system. The physical properties of the designed microparticles are investigated and correlated with enhancement in the imaging efficiency by experimental observation and theoretical interpretation. The X-ray absorption ability of the designed microparticle is assessed by Beer-Lambert-Bouguer law. Particle size, either in dried state or in solvent, primarily dominates the X-ray absorption ability under the given condition, thus affecting imaging efficiency of the designed X-ray contrast flow tracers. Copyright © 2011 John Wiley & Sons, Ltd.

X-ray source development for EXAFS measurements on the National Ignition Facility.

PubMed

Coppari, F; Thorn, D B; Kemp, G E; Craxton, R S; Garcia, E M; Ping, Y; Eggert, J H; Schneider, M B

2017-08-01

Extended X-ray absorption Fine Structure (EXAFS) measurements require a bright, spectrally smooth, and broad-band x-ray source. In a laser facility, such an x-ray source can be generated by a laser-driven capsule implosion. In order to optimize the x-ray emission, different capsule types and laser irradiations have been tested at the National Ignition Facility (NIF). A crystal spectrometer is used to disperse the x-rays and high efficiency image plate detectors are used to measure the absorption spectra in transmission geometry. EXAFS measurements at the K-edge of iron at ambient conditions have been obtained for the first time on the NIF laser, and the requirements for optimization have been established.

Differential phase contrast with a segmented detector in a scanning X-ray microprobe

PubMed Central

Hornberger, B.; de Jonge, M. D.; Feser, M.; Holl, P.; Holzner, C.; Jacobsen, C.; Legnini, D.; Paterson, D.; Rehak, P.; Strüder, L.; Vogt, S.

2008-01-01

Scanning X-ray microprobes are unique tools for the nanoscale investigation of specimens from the life, environmental, materials and other fields of sciences. Typically they utilize absorption and fluorescence as contrast mechanisms. Phase contrast is a complementary technique that can provide strong contrast with reduced radiation dose for weakly absorbing structures in the multi-keV range. In this paper the development of a segmented charge-integrating silicon detector which provides simultaneous absorption and differential phase contrast is reported. The detector can be used together with a fluorescence detector for the simultaneous acquisition of transmission and fluorescence data. It can be used over a wide range of photon energies, photon rates and exposure times at third-generation synchrotron radiation sources, and is currently operating at two beamlines at the Advanced Photon Source. Images obtained at around 2 keV and 10 keV demonstrate the superiority of phase contrast over absorption for specimens composed of light elements. PMID:18552427

Annealing induced atomic rearrangements on (Ga,In) (N,As) probed by hard X-ray photoelectron spectroscopy and X-ray absorption fine structure.

PubMed

Ishikawa, Fumitaro; Higashi, Kotaro; Fuyuno, Satoshi; Morifuji, Masato; Kondow, Masahiko; Trampert, Achim

2018-04-13

We study the effects of annealing on (Ga 0.64 ,In 0.36 ) (N 0.045 ,As 0.955 ) using hard X-ray photoelectron spectroscopy and X-ray absorption fine structure measurements. We observed surface oxidation and termination of the N-As bond defects caused by the annealing process. Specifically, we observed a characteristic chemical shift towards lower binding energies in the photoelectron spectra related to In. This phenomenon appears to be caused by the atomic arrangement, which produces increased In-N bond configurations within the matrix, as indicated by the X-ray absorption fine structure measurements. The reduction in the binding energies of group-III In, which occurs concomitantly with the atomic rearrangements of the matrix, causes the differences in the electronic properties of the system before and after annealing.

Local structure in LaMnO3 and CaMnO3 perovskites: A quantitative structural refinement of Mn K -edge XANES data

NASA Astrophysics Data System (ADS)

Monesi, C.; Meneghini, C.; Bardelli, F.; Benfatto, M.; Mobilio, S.; Manju, U.; Sarma, D. D.

2005-11-01

Hole-doped perovskites such as La1-xCaxMnO3 present special magnetic and magnetotransport properties, and it is commonly accepted that the local atomic structure around Mn ions plays a crucial role in determining these peculiar features. Therefore experimental techniques directly probing the local atomic structure, like x-ray absorption spectroscopy (XAS), have been widely exploited to deeply understand the physics of these compounds. Quantitative XAS analysis usually concerns the extended region [extended x-ray absorption fine structure (EXAFS)] of the absorption spectra. The near-edge region [x-ray absorption near-edge spectroscopy (XANES)] of XAS spectra can provide detailed complementary information on the electronic structure and local atomic topology around the absorber. However, the complexity of the XANES analysis usually prevents a quantitative understanding of the data. This work exploits the recently developed MXAN code to achieve a quantitative structural refinement of the Mn K -edge XANES of LaMnO3 and CaMnO3 compounds; they are the end compounds of the doped manganite series LaxCa1-xMnO3 . The results derived from the EXAFS and XANES analyses are in good agreement, demonstrating that a quantitative picture of the local structure can be obtained from XANES in these crystalline compounds. Moreover, the quantitative XANES analysis provides topological information not directly achievable from EXAFS data analysis. This work demonstrates that combining the analysis of extended and near-edge regions of Mn K -edge XAS spectra could provide a complete and accurate description of Mn local atomic environment in these compounds.

Investigating the local structure of B-site cations in (1-x)BaTiO3-xBiScO3 and (1-x)PbTiO3-xBiScO3 using X-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Blanchard, Peter E. R.; Grosvenor, Andrew P.

2018-05-01

The structural properties of (1-x)BaTiO3-xBiScO3 and (1-x)PbTiO3-xBiScO3 were investigated using powder X-ray diffraction and X-ray absorption spectroscopy. Diffraction measurements confirmed that substituting small amounts of BiScO3 into BaTiO3 initially stabilizes a cubic phase at x = 0.2 before impurity phases begin to form at x = 0.5. BiScO3 substitution also resulted in noticeable changes in the local coordination environment of Ti4+. X-ray absorption near-edge spectroscopy (XANES) analysis showed that replacing Ti4+ with Sc3+ results in an increase in the off-centre displacement of Ti4+ cations. Surprisingly, BiScO3 substitution has no effect on the displacement of the Ti4+ cation in the (1-x)PbTiO3-xBiScO3 solid solution.

Nanoparticle-enhanced x-ray therapy for cancer

NASA Astrophysics Data System (ADS)

Letfullin, Renat R.; Rice, Colin E. W.; George, Thomas F.

2016-03-01

Photothermal therapies of nanophotohyperthermia and nanophotothermolysis utilize the light absorptive properties of nanoparticles to create heat and free radicals in a small localized region. Conjugating nanoparticles with various biomolecules allows for targeted delivery to specific tissues or even specific cells, cancerous cells being of particular interest. Previous studies have investigated nanoparticles at visible and infrared wavelengths where surface plasmon resonance leads to unique absorption characteristics. However, issues such as poor penetration depth of the visible light through biological tissues limits the effectiveness of delivery by noninvasive means. In other news, various nanoparticles have been investigated as contrast agents for traditional X-ray procedures, utilizing the strong absorption characteristics of the nanoparticles to enhance contrast of the detected X-ray image. Using X-rays to power photothermal therapies has three main advantages over visiblespectra wavelengths: the high penetration depth of X-rays through biological media makes noninvasive treatments very feasible; the high energy of individual photons means nanoparticles can be heated to desired temperatures with lower beam intensities, or activated to produce the free radicals; and X-ray sources are already common throughout the medical industry, making future implementation on existing equipment possible. This paper uses Lorenz-Mie theory to investigate the light absorption properties of various size gold nanoparticles over photon energies in the 1-100 keV range. These absorption values are then plugged into a thermal model to determine the temperatures reached by the nanoparticles for X-ray exposures of differing time and intensity. The results of these simulations are discussed in relation to the effective implementation of nanophotohyperthermia and nanophotothermolysis treatments.

Dual-energy x-ray image decomposition by independent component analysis

NASA Astrophysics Data System (ADS)

Jiang, Yifeng; Jiang, Dazong; Zhang, Feng; Zhang, Dengfu; Lin, Gang

2001-09-01

The spatial distributions of bone and soft tissue in human body are separated by independent component analysis (ICA) of dual-energy x-ray images. It is because of the dual energy imaging modelí-s conformity to the ICA model that we can apply this method: (1) the absorption in body is mainly caused by photoelectric absorption and Compton scattering; (2) they take place simultaneously but are mutually independent; and (3) for monochromatic x-ray sources the total attenuation is achieved by linear combination of these two absorption. Compared with the conventional method, the proposed one needs no priori information about the accurate x-ray energy magnitude for imaging, while the results of the separation agree well with the conventional one.

Cobalt Distribution and Speciation: Effect of Aging, Intermittent Submergence, In situ Rice Roots

EPA Science Inventory

The speciation and distribution of cobalt (Co) in soils is poorly understood. This study was conducted using X-ray absorption spectroscopy (XAS) techniques to examine the influence of soluble Co(II) aging, submergence-dried cycling, and the presence of in vivo rice roots on the...

K- and L-edge X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) determination of differential orbital covalency (DOC) of transition metal sites

DOE PAGES

Baker, Michael L.; Mara, Michael W.; Yan, James J.; ...

2017-02-09

Continual advancements in the development of synchrotron radiation sources have resulted in X-ray based spectroscopic techniques capable of probing the electronic and structural properties of numerous systems. This review gives an overview of the application of metal K-edge and L-edge X-ray absorption spectroscopy (XAS), as well as Kα resonant inelastic X-ray scattering (RIXS), to the study of electronic structure in transition metal sites with emphasis on experimentally quantifying 3d orbital covalency. The specific sensitivities of K-edge XAS, L-edge XAS, and RIXS are discussed emphasizing the complementary nature of the methods. L-edge XAS and RIXS are sensitive to mixing between 3dmore » orbitals and ligand valence orbitals, and to the differential orbital covalency (DOC), that is, the difference in the covalencies for different symmetry sets of the d orbitals. Both L-edge XAS and RIXS are highly sensitive to and enable separation of σ and π donor bonding and π back bonding contributions to bonding. Applying ligand field multiplet simulations, including charge transfer via valence bond configuration interactions, DOC can be obtained for direct comparison with density functional theory calculations and to understand chemical trends. Here, the application of RIXS as a probe of frontier molecular orbitals in a heme enzyme demonstrates the potential of this method for the study of metal sites in highly covalent coordination sites in bioinorganic chemistry.« less

K- and L-edge X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) determination of differential orbital covalency (DOC) of transition metal sites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baker, Michael L.; Mara, Michael W.; Yan, James J.

Continual advancements in the development of synchrotron radiation sources have resulted in X-ray based spectroscopic techniques capable of probing the electronic and structural properties of numerous systems. This review gives an overview of the application of metal K-edge and L-edge X-ray absorption spectroscopy (XAS), as well as Kα resonant inelastic X-ray scattering (RIXS), to the study of electronic structure in transition metal sites with emphasis on experimentally quantifying 3d orbital covalency. The specific sensitivities of K-edge XAS, L-edge XAS, and RIXS are discussed emphasizing the complementary nature of the methods. L-edge XAS and RIXS are sensitive to mixing between 3dmore » orbitals and ligand valence orbitals, and to the differential orbital covalency (DOC), that is, the difference in the covalencies for different symmetry sets of the d orbitals. Both L-edge XAS and RIXS are highly sensitive to and enable separation of σ and π donor bonding and π back bonding contributions to bonding. Applying ligand field multiplet simulations, including charge transfer via valence bond configuration interactions, DOC can be obtained for direct comparison with density functional theory calculations and to understand chemical trends. Here, the application of RIXS as a probe of frontier molecular orbitals in a heme enzyme demonstrates the potential of this method for the study of metal sites in highly covalent coordination sites in bioinorganic chemistry.« less

THE IMPACT OF ACCURATE EXTINCTION MEASUREMENTS FOR X-RAY SPECTRAL MODELS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, Randall K.; Valencic, Lynne A.; Corrales, Lia, E-mail: lynne.a.valencic@nasa.gov

Interstellar extinction includes both absorption and scattering of photons from interstellar gas and dust grains, and it has the effect of altering a source's spectrum and its total observed intensity. However, while multiple absorption models exist, there are no useful scattering models in standard X-ray spectrum fitting tools, such as XSPEC. Nonetheless, X-ray halos, created by scattering from dust grains, are detected around even moderately absorbed sources, and the impact on an observed source spectrum can be significant, if modest, compared to direct absorption. By convolving the scattering cross section with dust models, we have created a spectral model asmore » a function of energy, type of dust, and extraction region that can be used with models of direct absorption. This will ensure that the extinction model is consistent and enable direct connections to be made between a source's X-ray spectral fits and its UV/optical extinction.« less

Monte Carlo analysis of megavoltage x-ray interaction-induced signal and noise in cadmium tungstate detectors for cargo container inspection

NASA Astrophysics Data System (ADS)

Kim, J.; Park, J.; Kim, J.; Kim, D. W.; Yun, S.; Lim, C. H.; Kim, H. K.

2016-11-01

For the purpose of designing an x-ray detector system for cargo container inspection, we have investigated the energy-absorption signal and noise in CdWO4 detectors for megavoltage x-ray photons. We describe the signal and noise measures, such as quantum efficiency, average energy absorption, Swank noise factor, and detective quantum efficiency (DQE), in terms of energy moments of absorbed energy distributions (AEDs) in a detector. The AED is determined by using a Monte Carlo simulation. The results show that the signal-related measures increase with detector thickness. However, the improvement of Swank noise factor with increasing thickness is weak, and this energy-absorption noise characteristic dominates the DQE performance. The energy-absorption noise mainly limits the signal-to-noise performance of CdWO4 detectors operated at megavoltage x-ray beam.

Vanadium K-edge X-ray absorption spectroscopy of bromoperoxidase from Ascophyllum nodosum

DOE Office of Scientific and Technical Information (OSTI.GOV)

Arber, J.M.; de Boer, E.; Garner, C.D.

Bromoperoxidase from Ascophyllum nodusum was the first vanadium-containing enzyme to be isolated. X-ray absorption spectra have now been collected in order to investigate the coordination of vanadium in the native, native plus bromide, native plus hydrogen peroxide, and dithionite-reduced forms of the enzyme. The edge and X-ray absorption near-edge structures show that, in the four samples studied, it is only on reduction of the native enzyme that the metal site is substantially altered. In addition, these data are consistent with the presence of vanadium(IV) in the reduced enzyme and vanadium(V) in the other samples. Extended X-ray absorption fine structure datamore » confirm that there are structural changes at the metal site on reduction of the native enzyme, notably a lengthening of the average inner-shell distance, and the presence of terminal oxygen together with histidine and oxygen-donating residues.« less

The origin of luminescence from di[4-(4-diphenylaminophenyl)phenyl]sulfone (DAPSF), a blue light emitter: an X-ray excited optical luminescence (XEOL) and X-ray absorption near edge structure (XANES) study.

PubMed

Zhang, Duo; Zhang, Hui; Zhang, Xiaohong; Sham, Tsun-Kong; Hu, Yongfeng; Sun, Xuhui

2016-03-07

The electronic structure and optical properties of di[4-(4-diphenylaminophenyl)phenyl]sulfone (denoted as DAPSF), a highly efficient fluorophor, have been investigated using X-ray excited optical luminescence (XEOL) and X-ray absorption near edge structure (XANES) spectroscopy at excitation energies across the C, N, O K-edges and the sulfur K-edge. The results indicate that the blue luminescence is mainly related to the sulfur functional group.

X-ray biosignature of bacteria in terrestrial and extra-terrestrial rocks

NASA Astrophysics Data System (ADS)

Lemelle, L.; Simionovici, A.; Susini, J.; Oger, P.; Chukalina, M.; Rau, Ch.; Golosio, B.; Gillet, P.

2003-04-01

X-ray imaging techniques at the best spatial resolution and using synchrotron facilities are put forth as powerful techniques for the search of small life forms in extraterrestrial rocks under quarantine conditions (Lemelle et al. 2003). Samples, which may be collected in situ on the martian surface or on a cometary surface, will be brought back and finally stored in a container. We tested on the ID22 beamline, the possibilities of the X-ray absorption and fluorescence tomographies on sub-mm grains of NWA817 (Lemelle et al. submitted) and Tatahouine (Simionovici et al. 2001) meteorites stored in a 10 micrometer silica capillary, full of air, mimicking such containers. Studies of the X-ray microtomographies carried on reveal the positions, the 3D textures and mineralogies of the microenvironments where traces of life should be looked for in priority (with a submicrometer spatial resolution). Limitations with respect to bacterial detection are due to the difficulties to obtain information about light elements (Z <= 14), major constituents of biological and silicate samples. At this stage, traces of life were not detected, nor identified such as, on all the studied meteorites through the capillary. Theoretical developments of an internal elemental microanalysis combining X-ray fluorescence, Compton and Transmission tomographies will soon allow improvements of 3D detection of life by X-ray techniques (Golosio et al. submitted). We tested on the ID21 beamline, the possibilities of the X-ray imaging techniques on bacteria/silicate assemblages prepared in the laboratory and directly placed in the beam. The X-ray signature of a "present" bacteria on a silicate surface was defined by X-ray mapping, out of a container, as coincident micrometer and oval zones having strong P and S fluorescence lines (S-fluorescence being slightly lower than P-fluorescence) and an amino-linked sulfur redox speciation. The X-ray signature of a single bacteria can now be applied to test the bacterial origin of nanostructures observed on some meteorite surfaces. Lemelle et al. (2003a) accepted to Journal de Physique, b submitted to Am. Min., Simionovici et al. (2001) Proc. SPIE, vol 4503, ed. U. BONSE, San Diego, August. Golosio et al. submitted to Phys. Rev. B

Nonlinear optical characterization of ZnS thin film synthesized by chemical spray pyrolysis method

NASA Astrophysics Data System (ADS)

G, Sreeja V.; V, Sabitha P.; Anila, E. I.; R, Reshmi; John, Manu Punnan; Radhakrishnan, P.

2014-10-01

ZnS thin film was prepared by Chemical Spray Pyrolysis (CSP) method. The sample was characterized by X-ray diffraction method and Z scan technique. XRD pattern showed that ZnS thin film has hexagonal structure with an average size of about 5.6nm. The nonlinear optical properties of ZnS thin film was studied by open aperture Z-Scan technique using Q-switched Nd-Yag Laser at 532nm. The Z-scan plot showed that the investigated ZnS thin film has saturable absorption behavior. The nonlinear absorption coefficient and saturation intensity were also estimated.

Determination of minor and trace elements in kidney stones by x-ray fluorescence analysis

NASA Astrophysics Data System (ADS)

Srivastava, Anjali; Heisinger, Brianne J.; Sinha, Vaibhav; Lee, Hyong-Koo; Liu, Xin; Qu, Mingliang; Duan, Xinhui; Leng, Shuai; McCollough, Cynthia H.

2014-03-01

The determination of accurate material composition of a kidney stone is crucial for understanding the formation of the kidney stone as well as for preventive therapeutic strategies. Radiations probing instrumental activation analysis techniques are excellent tools for identification of involved materials present in the kidney stone. In particular, x-ray fluorescence (XRF) can be very useful for the determination of minor and trace materials in the kidney stone. The X-ray fluorescence measurements were performed at the Radiation Measurements and Spectroscopy Laboratory (RMSL) of department of nuclear engineering of Missouri University of Science and Technology and different kidney stones were acquired from the Mayo Clinic, Rochester, Minnesota. Presently, experimental studies in conjunction with analytical techniques were used to determine the exact composition of the kidney stone. A new type of experimental set-up was developed and utilized for XRF analysis of the kidney stone. The correlation of applied radiation source intensity, emission of X-ray spectrum from involving elements and absorption coefficient characteristics were analyzed. To verify the experimental results with analytical calculation, several sets of kidney stones were analyzed using XRF technique. The elements which were identified from this techniques are Silver (Ag), Arsenic (As), Bromine (Br), Chromium (Cr), Copper (Cu), Gallium (Ga), Germanium (Ge), Molybdenum (Mo), Niobium (Nb), Rubidium (Rb), Selenium (Se), Strontium (Sr), Yttrium (Y), Zirconium (Zr). This paper presents a new approach for exact detection of accurate material composition of kidney stone materials using XRF instrumental activation analysis technique.

Histology-validated x-ray tomography for imaging human coronary arteries

NASA Astrophysics Data System (ADS)

Buscema, Marzia; Schulz, Georg; Deyhle, Hans; Khimchenko, Anna; Matviykiv, Sofiya; Holme, Margaret N.; Hipp, Alexander; Beckmann, Felix; Saxer, Till; Michaud, Katarzyna; Müller, Bert

2016-10-01

Heart disease is the number one cause of death worldwide. To improve therapy and patient outcome, the knowledge of anatomical changes in terms of lumen morphology and tissue composition of constricted arteries is crucial for designing a localized drug delivery to treat atherosclerosis disease. Traditional tissue characterization by histology is a pivotal tool, although it brings disadvantages such as vessel morphology modification during decalcification and slicing. X-ray tomography in absorption and phase contrast modes yields a deep understanding in blood vessel anatomy in healthy and diseased stages: measurements in absorption mode make visible highly absorbing tissue components including cholesterol plaques, whereas phase contrast tomography gains better contrast of the soft tissue components such as vessel walls. Established synchrotron radiation-based micro-CT techniques ensure high performance in terms of 3D visualization of highly absorbing and soft tissues.

Effect of reflection and refraction on NEXAFS spectra measured in TEY mode

PubMed Central

2018-01-01

The evolution of near-edge X-ray absorption fine structure in the vicinity of the K-absorption edge of oxygen for HfO2 over a wide range of incidence angles is analyzed by simultaneous implementation of the total-electron-yield (TEY) method and X-ray reflection spectroscopy. It is established that the effect of refraction on the TEY spectrum is greater than that of reflection and extends into the angular region up to angles 2θc. Within angles that are less than the critical angle, both the reflection and refraction strongly distort the shape of the TEY spectrum. Limitations of the technique for the calculation of optical constants from the reflection spectra using the Kramers–Kronig relation in the limited energy region in the vicinity of thresholds are discussed in detail. PMID:29271772

Origin of improved scintillation efficiency in (Lu,Gd)3(Ga,Al)5O12:Ce multicomponent garnets: An X-ray absorption near edge spectroscopy study

NASA Astrophysics Data System (ADS)

Wu, Yuntao; Luo, Jialiang; Nikl, Martin; Ren, Guohao

2014-01-01

In the recent successful improvement of scintillation efficiency in Lu3Al5O12:Ce driven by Ga3+ and Gd3+ admixture, the "band-gap engineering" and energy level positioning have been considered the valid strategies so far. This study revealed that this improvement was also associated with the cerium valence instability along with the changes of chemical composition. By utilizing X-ray absorption near edge spectroscopy technique, tuning the Ce3+/Ce4+ ratio by Ga3+ admixture was evidenced, while it was kept nearly stable with the Gd3+ admixture. Ce valence instability and Ce3+/Ce4+ ratio in multicomponent garnets can be driven by the energy separation between 4f ground state of Ce3+ and Fermi level.

Formation of nanostructures in Eu3+ doped glass-ceramics: an XAS study.

PubMed

Pellicer-Porres, J; Segura, A; Martínez-Criado, G; Rodríguez-Mendoza, U R; Lavín, V

2013-01-16

We describe the results of x-ray absorption experiments carried out to deduce structural and chemical information in Eu(3+) doped, transparent, oxyfluoride glass and nanostructured glass-ceramic samples. The spectra were measured at the Pb and Eu-L(III) edges. The Eu environment in the glass samples is observed to be similar to that of EuF(3). Complementary x-ray diffraction experiments show that thermal annealing creates β-PbF(2) type nanocrystals. X-ray absorption indicates that Eu ions act as seeds in the nanocrystal formation. There is evidence of interstitial fluorine atoms around Eu ions as well as Eu dimers. X-ray absorption at the Pb-L(III) edge shows that after the thermal treatment most lead atoms form a PbO amorphous phase and that only 10% of the lead atoms remain available to form β-PbF(2) type nanocrystals. Both x-ray diffraction and absorption point to a high Eu content in the nanocrystals. Our study suggests new approaches to the oxyfluoride glass-ceramic synthesis in order to further improve their properties.

Alternative difference analysis scheme combining R -space EXAFS fit with global optimization XANES fit for X-ray transient absorption spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhan, Fei; Tao, Ye; Zhao, Haifeng

Time-resolved X-ray absorption spectroscopy (TR-XAS), based on the laser-pump/X-ray-probe method, is powerful in capturing the change of the geometrical and electronic structure of the absorbing atom upon excitation. TR-XAS data analysis is generally performed on the laser-on minus laser-off difference spectrum. Here, a new analysis scheme is presented for the TR-XAS difference fitting in both the extended X-ray absorption fine-structure (EXAFS) and the X-ray absorption near-edge structure (XANES) regions.R-space EXAFS difference fitting could quickly provide the main quantitative structure change of the first shell. The XANES fitting part introduces a global non-derivative optimization algorithm and optimizes the local structure changemore » in a flexible way where both the core XAS calculation package and the search method in the fitting shell are changeable. The scheme was applied to the TR-XAS difference analysis of Fe(phen) 3spin crossover complex and yielded reliable distance change and excitation population.« less

Simulation of X-ray transient absorption for following vibrations in coherently ionized F2 molecules

NASA Astrophysics Data System (ADS)

Dutoi, Anthony D.; Leone, Stephen R.

2017-01-01

Femtosecond and attosecond X-ray transient absorption experiments are becoming increasingly sophisticated tools for probing nuclear dynamics. In this work, we explore and develop theoretical tools needed for interpretation of such spectra,in order to characterize the vibrational coherences that result from ionizing a molecule in a strong IR field. Ab initio data for F2 is combined with simulations of nuclear dynamics, in order to simulate time-resolved X-ray absorption spectra for vibrational wavepackets after coherent ionization at 0 K and at finite temperature. Dihalogens pose rather difficult electronic structure problems, and the issues encountered in this work will be reflective of those encountered with any core-valence excitation simulation when a bond is breaking. The simulations reveal a strong dependence of the X-ray absorption maximum on the locations of the vibrational wave packets. A Fourier transform of the simulated signal shows features at the overtone frequencies of both the neutral and the cation, which reflect spatial interferences of the vibrational eigenstates. This provides a direct path for implementing ultrafast X-ray spectroscopic methods to visualize coherent nuclear dynamics.

Alternative difference analysis scheme combining R-space EXAFS fit with global optimization XANES fit for X-ray transient absorption spectroscopy.

PubMed

Zhan, Fei; Tao, Ye; Zhao, Haifeng

2017-07-01

Time-resolved X-ray absorption spectroscopy (TR-XAS), based on the laser-pump/X-ray-probe method, is powerful in capturing the change of the geometrical and electronic structure of the absorbing atom upon excitation. TR-XAS data analysis is generally performed on the laser-on minus laser-off difference spectrum. Here, a new analysis scheme is presented for the TR-XAS difference fitting in both the extended X-ray absorption fine-structure (EXAFS) and the X-ray absorption near-edge structure (XANES) regions. R-space EXAFS difference fitting could quickly provide the main quantitative structure change of the first shell. The XANES fitting part introduces a global non-derivative optimization algorithm and optimizes the local structure change in a flexible way where both the core XAS calculation package and the search method in the fitting shell are changeable. The scheme was applied to the TR-XAS difference analysis of Fe(phen) 3 spin crossover complex and yielded reliable distance change and excitation population.

Weak hard X-ray emission from broad absorption line quasars: evidence for intrinsic X-ray weakness

DOE Office of Scientific and Technical Information (OSTI.GOV)

Luo, B.; Brandt, W. N.; Scott, A. E.

We report NuSTAR observations of a sample of six X-ray weak broad absorption line (BAL) quasars. These targets, at z = 0.148-1.223, are among the optically brightest and most luminous BAL quasars known at z < 1.3. However, their rest-frame ≈2 keV luminosities are 14 to >330 times weaker than expected for typical quasars. Our results from a pilot NuSTAR study of two low-redshift BAL quasars, a Chandra stacking analysis of a sample of high-redshift BAL quasars, and a NuSTAR spectral analysis of the local BAL quasar Mrk 231 have already suggested the existence of intrinsically X-ray weak BAL quasars,more » i.e., quasars not emitting X-rays at the level expected from their optical/UV emission. The aim of the current program is to extend the search for such extraordinary objects. Three of the six new targets are weakly detected by NuSTAR with ≲ 45 counts in the 3-24 keV band, and the other three are not detected. The hard X-ray (8-24 keV) weakness observed by NuSTAR requires Compton-thick absorption if these objects have nominal underlying X-ray emission. However, a soft stacked effective photon index (Γ{sub eff} ≈ 1.8) for this sample disfavors Compton-thick absorption in general. The uniform hard X-ray weakness observed by NuSTAR for this and the pilot samples selected with <10 keV weakness also suggests that the X-ray weakness is intrinsic in at least some of the targets. We conclude that the NuSTAR observations have likely discovered a significant population (≳ 33%) of intrinsically X-ray weak objects among the BAL quasars with significantly weak <10 keV emission. We suggest that intrinsically X-ray weak quasars might be preferentially observed as BAL quasars.« less

Lithographically fabricated silicon microreactor for in situ characterization of heterogeneous catalysts—Enabling correlative characterization techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baier, S.; Rochet, A.; Hofmann, G.

2015-06-15

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The silicon microreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy. Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor formore » in situ studies.« less

Phase contrast imaging of cochlear soft tissue.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, S.; Hwang, M.; Rau, C.

A noninvasive technique to image soft tissue could expedite diagnosis and disease management in the auditory system. We propose inline phase contrast imaging with hard X-rays as a novel method that overcomes the limitations of conventional absorption radiography for imaging soft tissue. In this study, phase contrast imaging of mouse cochleae was performed at the Argonne National Laboratory Advanced Photon Source. The phase contrast tomographic reconstructions show soft tissue structures of the cochlea, including the inner pillar cells, the inner spiral sulcus, the tectorial membrane, the basilar membrane, and the Reissner's membrane. The results suggest that phase contrast X-ray imagingmore » and tomographic techniques hold promise to noninvasively image cochlear structures at an unprecedented cellular level.« less

Space Telescope and Optical Reverberation Mapping Project VI. Variations of the Intrinsic Absorption Lines in NGC 5548

NASA Astrophysics Data System (ADS)

Kriss, Gerard A.; Agn Storm Team

2015-01-01

The AGN STORM collaboration monitored the Seyfert 1 galaxy NGC 5548 over a six-month period, with observations spanning the hard X-ray to mid-infrared wavebands. The core of this campaign was an intensive HST COS program, which obtained 170 far-ultraviolet spectra at approximately daily intervals, with twice-per-day monitoring of the X-ray, near-UV, and optical bands during much of the same period using Swift. The broad UV absorption lines discovered by Kaastra et al. (2014) and associated with the new soft X-ray obscurer are continuously present in the STORM campaign COS spectra. Their strength varies with the degree of soft X-ray obscuration as revealed by the Swift X-ray spectra. The narrow associated absorption lines in the UV spectrum of NGC 5548 remain strong. The lower-ionization transitions that appeared concurrently with the soft X-ray obscuration vary in response to the changing UV flux on a daily basis. Their depths over the longer term, however, also respond to the strength of the soft X-ray obscuration, indicating that the soft X-ray obscurer has a significant influence on the ionizing UV continuum that is not directly tracked by the observable UV continuum itself.

Development of a spectro-electrochemical cell for soft X-ray photon-in photon-out spectroscopy

NASA Astrophysics Data System (ADS)

Ishihara, Tomoko; Tokushima, Takashi; Horikawa, Yuka; Kato, Masaru; Yagi, Ichizo

2017-10-01

We developed a spectro-electrochemical cell for X-ray absorption and X-ray emission spectroscopy, which are element-specific methods to study local electronic structures in the soft X-ray region. In the usual electrochemical measurement setup, the electrode is placed in solution, and the surface/interface region of the electrode is not normally accessible by soft X-rays that have low penetration depth in liquids. To realize soft X-ray observation of electrochemical reactions, a 15-nm-thick Pt layer was deposited on a 150-nm-thick film window with an adhesive 3-nm-thick Ti layer for use as both the working electrode and the separator window between vacuum and a sample liquid under atmospheric pressure. The designed three-electrode electrochemical cell consists of a Pt film on a SiC window, a platinized Pt wire, and a commercial Ag|AgCl electrode as the working, counter, and reference electrodes, respectively. The functionality of the cell was tested by cyclic voltammetry and X-ray absorption and emission spectroscopy. As a demonstration, the electroplating of Pb on the Pt/SiC membrane window was measured by X-ray absorption and real-time monitoring of fluorescence intensity at the O 1s excitation.

Electrooptic crystal growth and properties

NASA Astrophysics Data System (ADS)

1994-02-01

A new member in the tungsten-bronze family of ferroelectric lead potassium niobate (PKN), with general formula Pb(1-x)K(2x)Nb2O6, has been grown as bulk single crystal. Growth of PKN with charge composition x = 0.23 has been achieved using the Czochralski technique of crystal pulling. Large diameter boules were grown in platinum crucibles at temperatures between 1280 and 1300 C. Crystallographic studies were conducted using x ray diffraction techniques. The samples were characterized for ferroelectric properties between 25 and 600 C and for optical absorption. This paper presents the crystal synthesis and the results of ferroelectric and optical characterization. Bulk single crystals of potassium tantalate niobate, KTa(1-x)Nb(x)O3, ferroelectric with different values of Ta/Nb ratios have been grown by temperature gradient transport technique (TGTT). A second attached paper presents the results of the crystal growth experiments, ferroelectric characterization techniques, and properties of potassium tantalate niobate crystals.

Innovative combination of spectroscopic techniques to reveal nanoparticle fate in a crop plant

NASA Astrophysics Data System (ADS)

Larue, Camille; Castillo-Michel, Hiram; Stein, Ricardo J.; Fayard, Barbara; Pouyet, Emeline; Villanova, Julie; Magnin, Valérie; Pradas del Real, Ana-Elena; Trcera, Nicolas; Legros, Samuel; Sorieul, Stéphanie; Sarret, Géraldine

2016-05-01

Nanotechnology is the new industrial revolution of our century. Its development leads to an increasing use of nanoparticles and thus to their dissemination. Their fate in the environment is of great concern and especially their possible transfer in trophic chains might be an issue for food safety. However, so far our knowledge on this topic has been restricted by the lack of appropriate techniques to characterize their behavior in complex matrices. Here, we present in detail the use of cutting-edge beam-based techniques for nanoparticle in situ localization, quantification and speciation in a crop plant species (Lactuca sativa). Lettuce seedlings have been exposed to TiO2 and Ag nanoparticles and analyzed by inductively coupled plasma spectrometry, micro-particle induced X-ray emission coupled to Rutherford backscattering spectroscopy on nuclear microprobe, micro-X-ray fluorescence spectroscopy and X-ray absorption near edge structure spectroscopy. The benefits and drawbacks of each technique are discussed, and the types of information that can be drawn, for example on the translocation to edible parts, change of speciation within the plant, detoxification mechanisms, or impact on the plant ionome, are highlighted. Such type of coupled approach would be an asset for nanoparticle risk assessment.

Structure of Nano-sized CeO 2 Materials: Combined Scattering and Spectroscopic Investigations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Marchbank, Huw R.; Clark, Adam H.; Hyde, Timothy I.

Here, the nature of nano-sized ceria, CeO 2, systems were investigated using neutron and X-ray diffraction and X-ray absorption spectroscopy. Whilst both diffraction andtotal pair distribution functions (PDFs) revealed that in all the samples the occupancy of both Ce 4+ and O 2- are very close to the ideal stoichiometry, the analysis using reverse Monte Carlo technique revealedsignificant disorder around oxygen atoms in the nano sized ceria samples in comparison to the highly crystalline NIST standard.In addition, the analysis reveal that the main differences observed in the pair correlations from various X-ray and neutron diffraction techniques were attributed to themore » particle size of the CeO 2 prepared by the reported three methods. Furthermore, detailed analysis of the Ce L 3– and K-edge EXAFS data support this finding; in particular the decrease in higher shell coordination numbers with respect to the NIST standard, are attributed to differences in particle size.« less

Structure of Nano-sized CeO 2 Materials: Combined Scattering and Spectroscopic Investigations

DOE PAGES

Marchbank, Huw R.; Clark, Adam H.; Hyde, Timothy I.; ...

2016-08-29

Here, the nature of nano-sized ceria, CeO 2, systems were investigated using neutron and X-ray diffraction and X-ray absorption spectroscopy. Whilst both diffraction andtotal pair distribution functions (PDFs) revealed that in all the samples the occupancy of both Ce 4+ and O 2- are very close to the ideal stoichiometry, the analysis using reverse Monte Carlo technique revealedsignificant disorder around oxygen atoms in the nano sized ceria samples in comparison to the highly crystalline NIST standard.In addition, the analysis reveal that the main differences observed in the pair correlations from various X-ray and neutron diffraction techniques were attributed to themore » particle size of the CeO 2 prepared by the reported three methods. Furthermore, detailed analysis of the Ce L 3– and K-edge EXAFS data support this finding; in particular the decrease in higher shell coordination numbers with respect to the NIST standard, are attributed to differences in particle size.« less

K-edge subtraction synchrotron X-ray imaging in bio-medical research.

PubMed

Thomlinson, W; Elleaume, H; Porra, L; Suortti, P

2018-05-01

High contrast in X-ray medical imaging, while maintaining acceptable radiation dose levels to the patient, has long been a goal. One of the most promising methods is that of K-edge subtraction imaging. This technique, first advanced as long ago as 1953 by B. Jacobson, uses the large difference in the absorption coefficient of elements at energies above and below the K-edge. Two images, one taken above the edge and one below the edge, are subtracted leaving, ideally, only the image of the distribution of the target element. This paper reviews the development of the KES techniques and technology as applied to bio-medical imaging from the early low-power tube sources of X-rays to the latest high-power synchrotron sources. Applications to coronary angiography, functional lung imaging and bone growth are highlighted. A vision of possible imaging with new compact sources is presented. Copyright © 2018 Associazione Italiana di Fisica Medica. Published by Elsevier Ltd. All rights reserved.

Determining the Oxygen Fugacity of Lunar Pyroclastic Glasses Using Vanadium Valence - An Update

NASA Technical Reports Server (NTRS)

Karner, J. M.; Sutton, S. R.; Papike, J. J.; Shearer, C. K.; Jones, J. H.; Newville, M.

2004-01-01

We have been developing an oxygen barometer based on the valence state of V (V(2+), V(3+), V(4+), and V(5+)) in solar system basaltic glasses. The V valence is determined by synchrotron micro x-ray absorption near edge structure (XANES), which uses x-ray absorption associated with core-electronic transitions (absorption edges) to reveal a pre-edge peak whose intensity is directly proportional to the valence state of an element. XANES has advantages over other techniques that determine elemental valence because measurements can be made non-destructively in air and in situ on conventional thin sections at a micrometer spatial resolution with elemental sensitivities of approx. 100 ppm. Recent results show that fO2 values derived from the V valence technique are consistent with fO2 estimates determined by other techniques for materials that crystallized above the IW buffer. The fO2's determined by V valence (IW-3.8 to IW-2) for the lunar pyroclastic glasses, however, are on the order of 1 to 2.8 log units below previous estimates. Furthermore, the calculated fO2's decrease with increasing TiO2 contents from the A17 VLT to the A17 Orange glasses. In order to investigate these results further, we have synthesized lunar green and orange glasses and examined them by XANES.

Excited state X-ray absorption spectroscopy: Probing both electronic and structural dynamics

NASA Astrophysics Data System (ADS)

Neville, Simon P.; Averbukh, Vitali; Ruberti, Marco; Yun, Renjie; Patchkovskii, Serguei; Chergui, Majed; Stolow, Albert; Schuurman, Michael S.

2016-10-01

We investigate the sensitivity of X-ray absorption spectra, simulated using a general method, to properties of molecular excited states. Recently, Averbukh and co-workers [M. Ruberti et al., J. Chem. Phys. 140, 184107 (2014)] introduced an efficient and accurate L 2 method for the calculation of excited state valence photoionization cross-sections based on the application of Stieltjes imaging to the Lanczos pseudo-spectrum of the algebraic diagrammatic construction (ADC) representation of the electronic Hamiltonian. In this paper, we report an extension of this method to the calculation of excited state core photoionization cross-sections. We demonstrate that, at the ADC(2)x level of theory, ground state X-ray absorption spectra may be accurately reproduced, validating the method. Significantly, the calculated X-ray absorption spectra of the excited states are found to be sensitive to both geometric distortions (structural dynamics) and the electronic character (electronic dynamics) of the initial state, suggesting that core excitation spectroscopies will be useful probes of excited state non-adiabatic dynamics. We anticipate that the method presented here can be combined with ab initio molecular dynamics calculations to simulate the time-resolved X-ray spectroscopy of excited state molecular wavepacket dynamics.

Synthesis and x-ray characterization of cobalt phosphide (Co₂P) nanorods for the oxygen reduction reaction

DOE PAGES

Doan-Nguyen, Vicky V.T.; Su, Dong; Zhang, Sen; ...

2015-07-14

Low temperature fuel cells are clean, effective alternative fuel conversion technology. Oxygen reduction reaction (ORR) at the fuel cell cathode has required Pt as the electrocatalyst for high activity and selectivity of the four-electron reaction pathway. Targeting a less expensive, earth abundant alternative, we have developed the synthesis of cobalt phosphide (Co₂P) nanorods for ORR. Characterization techniques that include total X-ray scattering and extended X-ray absorption fine structure revealed a deviation of the nanorods from bulk crystal structure with a contraction along the b orthorhombic lattice parameter. The carbon supported nanorods have comparable activity but are remarkably more stable thanmore » conventional Pt catalysts for the oxygen reduction reaction in alkaline environments.« less

Solution Structures of Highly Active Molecular Ir Water-Oxidation Catalysts from Density Functional Theory Combined with High-Energy X-ray Scattering and EXAFS Spectroscopy.

PubMed

Yang, Ke R; Matula, Adam J; Kwon, Gihan; Hong, Jiyun; Sheehan, Stafford W; Thomsen, Julianne M; Brudvig, Gary W; Crabtree, Robert H; Tiede, David M; Chen, Lin X; Batista, Victor S

2016-05-04

The solution structures of highly active Ir water-oxidation catalysts are elucidated by combining density functional theory, high-energy X-ray scattering (HEXS), and extended X-ray absorption fine structure (EXAFS) spectroscopy. We find that the catalysts are Ir dimers with mono-μ-O cores and terminal anionic ligands, generated in situ through partial oxidation of a common catalyst precursor. The proposed structures are supported by (1)H and (17)O NMR, EPR, resonance Raman and UV-vis spectra, electrophoresis, etc. Our findings are particularly valuable to understand the mechanism of water oxidation by highly reactive Ir catalysts. Importantly, our DFT-EXAFS-HEXS methodology provides a new in situ technique for characterization of active species in catalytic systems.

X-ray source development for EXAFS measurements on the National Ignition Facility

DOE PAGES

Coppari, F.; Thorn, D. B.; Kemp, G. E.; ...

2017-08-28

We present that extended X-ray absorption Fine Structure (EXAFS) measurements require a bright, spectrally smooth, and broad-band x-ray source. In a laser facility, such an x-ray source can be generated by a laser-driven capsule implosion. In order to optimize the x-ray emission, different capsule types and laser irradiations have been tested at the National Ignition Facility (NIF). A crystal spectrometer is used to disperse the x-rays and high efficiency image plate detectors are used to measure the absorption spectra in transmission geometry. Finally, EXAFS measurements at the K-edge of iron at ambient conditions have been obtained for the first timemore » on the NIF laser, and the requirements for optimization have been established.« less

Elemental and Molecular Segregation in Oil Paintings due to Lead Soap Degradation

DOE PAGES

Chen-Wiegart, Yu-chen Karen; Catalano, Jaclyn; Williams, Garth J.; ...

2017-09-14

The formation of Pb, Zn, and Cu carboxylates (soaps) has caused visible deterioration in hundreds of oil paintings dating from the 15th century to the present. Through transport phenomena not yet understood, free fatty acids in the oil binding medium migrate through the paint and react with pigments containing heavy metals to form soaps. To investigate the complex correlation among the elemental segregation, types of chemical compounds formed, and possible mechanisms of the reactions, a paint sample cross-section from a 15th century oil painting was examined by synchrotron X-ray techniques. X-ray fluorescence (XRF) microscopy, quantified with elemental correlation density distribution,more » showed Pb and Sn segregation in the soap-affected areas. X-ray absorption near edge structure (XANES) around the Pb-L3 absorption edge showed that Pb pigments and Pb soaps can be distinguished while micro-XANES gave further information on the chemical heterogeneity in the paint film. The advantages and limitations of these synchrotron-based techniques are discussed and compared to those of methods routinely used to analyze paint samples. The results presented set the stage for improving the information extracted from samples removed from works of art and for correlating observations in model paint samples to those in the naturally aged samples, to shed light onto the mechanism of soap formation.« less

Elemental and Molecular Segregation in Oil Paintings due to Lead Soap Degradation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen-Wiegart, Yu-chen Karen; Catalano, Jaclyn; Williams, Garth J.

The formation of Pb, Zn, and Cu carboxylates (soaps) has caused visible deterioration in hundreds of oil paintings dating from the 15th century to the present. Through transport phenomena not yet understood, free fatty acids in the oil binding medium migrate through the paint and react with pigments containing heavy metals to form soaps. To investigate the complex correlation among the elemental segregation, types of chemical compounds formed, and possible mechanisms of the reactions, a paint sample cross-section from a 15th century oil painting was examined by synchrotron X-ray techniques. X-ray fluorescence (XRF) microscopy, quantified with elemental correlation density distribution,more » showed Pb and Sn segregation in the soap-affected areas. X-ray absorption near edge structure (XANES) around the Pb-L3 absorption edge showed that Pb pigments and Pb soaps can be distinguished while micro-XANES gave further information on the chemical heterogeneity in the paint film. The advantages and limitations of these synchrotron-based techniques are discussed and compared to those of methods routinely used to analyze paint samples. The results presented set the stage for improving the information extracted from samples removed from works of art and for correlating observations in model paint samples to those in the naturally aged samples, to shed light onto the mechanism of soap formation.« less

High resolution, multiple-energy linear sweep detector for x-ray imaging

DOEpatents

Perez-Mendez, Victor; Goodman, Claude A.

1996-01-01

Apparatus for generating plural electrical signals in a single scan in response to incident X-rays received from an object. Each electrical signal represents an image of the object at a different range of energies of the incident X-rays. The apparatus comprises a first X-ray detector, a second X-ray detector stacked upstream of the first X-ray detector, and an X-ray absorber stacked upstream of the first X-ray detector. The X-ray absorber provides an energy-dependent absorption of the incident X-rays before they are incident at the first X-ray detector, but provides no absorption of the incident X-rays before they are incident at the second X-ray detector. The first X-ray detector includes a linear array of first pixels, each of which produces an electrical output in response to the incident X-rays in a first range of energies. The first X-ray detector also includes a circuit that generates a first electrical signal in response to the electrical output of each of the first pixels. The second X-ray detector includes a linear array of second pixels, each of which produces an electrical output in response to the incident X-rays in a second range of energies, broader than the first range of energies. The second X-ray detector also includes a circuit that generates a second electrical signal in response to the electrical output of each of the second pixels.

High resolution, multiple-energy linear sweep detector for x-ray imaging

DOEpatents

Perez-Mendez, V.; Goodman, C.A.

1996-08-20

Apparatus is disclosed for generating plural electrical signals in a single scan in response to incident X-rays received from an object. Each electrical signal represents an image of the object at a different range of energies of the incident X-rays. The apparatus comprises a first X-ray detector, a second X-ray detector stacked upstream of the first X-ray detector, and an X-ray absorber stacked upstream of the first X-ray detector. The X-ray absorber provides an energy-dependent absorption of the incident X-rays before they are incident at the first X-ray detector, but provides no absorption of the incident X-rays before they are incident at the second X-ray detector. The first X-ray detector includes a linear array of first pixels, each of which produces an electrical output in response to the incident X-rays in a first range of energies. The first X-ray detector also includes a circuit that generates a first electrical signal in response to the electrical output of each of the first pixels. The second X-ray detector includes a linear array of second pixels, each of which produces an electrical output in response to the incident X-rays in a second range of energies, broader than the first range of energies. The second X-ray detector also includes a circuit that generates a second electrical signal in response to the electrical output of each of the second pixels. 12 figs.

Two-photon absorption of soft X-ray free electron laser radiation by graphite near the carbon K-absorption edge

NASA Astrophysics Data System (ADS)

Lam, Royce K.; Raj, Sumana L.; Pascal, Tod A.; Pemmaraju, C. D.; Foglia, Laura; Simoncig, Alberto; Fabris, Nicola; Miotti, Paolo; Hull, Christopher J.; Rizzuto, Anthony M.; Smith, Jacob W.; Mincigrucci, Riccardo; Masciovecchio, Claudio; Gessini, Alessandro; De Ninno, Giovanni; Diviacco, Bruno; Roussel, Eleonore; Spampinati, Simone; Penco, Giuseppe; Di Mitri, Simone; Trovò, Mauro; Danailov, Miltcho B.; Christensen, Steven T.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Coreno, Marcello; Poletto, Luca; Drisdell, Walter S.; Prendergast, David; Giannessi, Luca; Principi, Emiliano; Nordlund, Dennis; Saykally, Richard J.; Schwartz, Craig P.

2018-07-01

We have examined the transmission of soft X-ray pulses from the FERMI free electron laser through carbon films of varying thickness, quantifying nonlinear effects of pulses above and below the carbon K-edge. At typical of soft X-ray free electron laser intensities, pulses exhibit linear absorption at photon energies above and below the K-edge, ∼308 and ∼260 eV, respectively; whereas two-photon absorption becomes significant slightly below the K-edge, ∼284.2 eV. The measured two-photon absorption cross section at 284.18 eV (∼6 × 10-48 cm4 s) is 7 orders of magnitude above what is expected from a simple theory based on hydrogen-like atoms - a result of resonance effects.

High resolution x-ray absorption and emission spectroscopy of Li x CoO2 single crystals as a function delithiation

NASA Astrophysics Data System (ADS)

Simonelli, L.; Paris, E.; Iwai, C.; Miyoshi, K.; Takeuchi, J.; Mizokawa, T.; Saini, N. L.

2017-03-01

The effect of delithiation in Li x CoO2 is studied by high resolution Co K-edge x-ray absorption and x-ray emission spectroscopy. Polarization dependence of the x-ray absorption spectra on single crystal samples is exploited to reveal information on the anisotropic electronic structure. We find that the electronic structure of Li x CoO2 is significantly affected by delithiation in which the Co ions oxidation state tending to change from 3+  to 4+. The Co intersite (intrasite) 4p-3d hybridization suffers a decrease (increase) by delithiation. The unoccupied 3d t 2g orbitals with a 1g symmetry, containing substantial O 2p character, hybridize isotropically with Co 4p orbitals and likely to have itinerant character unlike anisotropically hybridized 3d e g orbitals. Such a peculiar electronic structure could have significant effect on the mobility of Li in Li x CoO2 cathode and hence the battery characteristics.

Enhancing Tabletop X-Ray Phase Contrast Imaging with Nano-Fabrication

PubMed Central

Miao, Houxun; Gomella, Andrew A.; Harmon, Katherine J.; Bennett, Eric E.; Chedid, Nicholas; Znati, Sami; Panna, Alireza; Foster, Barbara A.; Bhandarkar, Priya; Wen, Han

2015-01-01

X-ray phase-contrast imaging is a promising approach for improving soft-tissue contrast and lowering radiation dose in biomedical applications. While current tabletop imaging systems adapt to common x-ray tubes and large-area detectors by employing absorptive elements such as absorption gratings or monolithic crystals to filter the beam, we developed nanometric phase gratings which enable tabletop x-ray far-field interferometry with only phase-shifting elements, leading to a substantial enhancement in the performance of phase contrast imaging. In a general sense the method transfers the demands on the spatial coherence of the x-ray source and the detector resolution to the feature size of x-ray phase masks. We demonstrate its capabilities in hard x-ray imaging experiments at a fraction of clinical dose levels and present comparisons with the existing Talbot-Lau interferometer and with conventional digital radiography. PMID:26315891

Erratum: Creation of X-Ray Transparency of Matter by Stimulated Elastic Forward Scattering [Phys. Rev. Lett. 115 , 107402 (2015)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stöhr, J.; Scherz, A.

X-ray absorption by matter has long been described by the famous Beer-Lambert law. Here we show how this fundamental law needs to be modified for high-intensity coherent x-ray pulses, now available at x-ray free electron lasers, due to the onset of stimulated elastic forward scattering. We present an analytical expression for the modified polarization-dependent Beer-Lambert law for the case of resonant core-to-valence electronic transitions and incident transform limited x-ray pulses. Upon transmission through a solid, the absorption and dichroic contrasts are found to vanish with increasing x-ray intensity, with the stimulation threshold lowered by orders of magnitude through a super-radiativemore » coherent effect. Our results have broad implications for the study of matter with x-ray lasers.« less

Hard X-ray tests of the unified model for an ultraviolet-detected sample of Seyfert 2 galaxies

NASA Technical Reports Server (NTRS)

Mulchaey, John S.; Myshotzky, Richard F.; Weaver, Kimberly A.

1992-01-01

An ultraviolet-detected sample of Seyfert 2 galaxies shows heavy photoelectric absorption in the hard X-ray band. The presence of UV emission combined with hard X-ray absorption argues strongly for a special geometry which must have the general properties of the Antonucci and Miller unified model. The observations of this sample are consistent with the picture in which the hard X-ray photons are viewed directly through the obscuring matter (molecular torus?) and the optical, UV, and soft X-ray continuum are seen in scattered light. The large range in X-ray column densities implies that there must be a large variation in intrinsic thicknesses of molecular tori, an assumption not found in the simplest of unified models. Furthermore, constraints based on the cosmic X-ray background suggest that some of the underlying assumptions of the unified model are wrong.

Characterization of ion-induced radiation effects in nuclear materials using synchrotron x-ray techniques

DOE PAGES

Lang, Maik; Tracy, Cameron L.; Palomares, Raul I.; ...

2015-05-01

Recent efforts to characterize the nanoscale structural and chemical modifications induced by energetic ion irradiation in nuclear materials have greatly benefited from the application of synchrotron-based x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS) techniques. Key to the study of actinide-bearing materials has been the use of small sample volumes, which are particularly advantageous, as the small quantities minimize the level of radiation exposure at the ion-beam and synchrotron user facility. This approach utilizes energetic heavy ions (energy range: 100 MeV–3 GeV) that pass completely through the sample thickness and deposit an almost constant energy per unit length along theirmore » trajectory. High energy x-rays (25–65 keV) from intense synchrotron light sources are then used in transmission geometry to analyze ion-induced structural and chemical modifications throughout the ion tracks. We describe in detail the experimental approach for utilizing synchrotron radiation (SR) to study the radiation response of a range of nuclear materials (e.g., ThO 2 and Gd 2Ti xZr 2–xO 7). Also addressed is the use of high-pressure techniques, such as the heatable diamond anvil cell, as a new means to expose irradiated materials to well-controlled high-temperature (up to 1000 °C) and/or high-pressure (up to 50 GPa) conditions. Furthermore, this is particularly useful for characterizing the annealing kinetics of irradiation-induced material modifications.« less

Mercury Speciation by X-ray Absorption Fine Structure Spectroscopy and Sequential Chemical Extractions: A Comparison of Speciation Methods

USGS Publications Warehouse

Kim, C.S.; Bloom, N.S.; Rytuba, J.J.; Brown, Gordon E.

2003-01-01

Determining the chemical speciation of mercury in contaminated mining and industrial environments is essential for predicting its solubility, transport behavior, and potential bioavailability as well as for designing effective remediation strategies. In this study, two techniques for determining Hg speciation-X-ray absorption fine structure (XAFS) spectroscopy and sequential chemical extractions (SCE)-are independently applied to a set of samples with Hg concentrations ranging from 132 to 7539 mg/kg to determine if the two techniques provide comparable Hg speciation results. Generally, the proportions of insoluble HgS (cinnabar, metacinnabar) and HgSe identified by XAFS correlate well with the proportion of Hg removed in the aqua regia extraction demonstrated to remove HgS and HgSe. Statistically significant (> 10%) differences are observed however in samples containing more soluble Hg-containing phases (HgCl2, HgO, Hg3S2O 4). Such differences may be related to matrix, particle size, or crystallinity effects, which could affect the apparent solubility of Hg phases present. In more highly concentrated samples, microscopy techniques can help characterize the Hg-bearing species in complex multiphase natural samples.

X ray absorption by dark nebulae (HEAO-2 guest investigator program)

NASA Technical Reports Server (NTRS)

Sanders, W. T.

1991-01-01

A study is described of data obtained from the Imaging Proportional Counter (IPC) x ray detector aboard the HEAO-2 satellite (Einstein Observatory). The research project involved a search for absorption of diffuse low energy x ray background emission by galactic dark nebulae. The commonly accepted picture that the bulk of the C band emission originates locally, closer that a few hundred parsec, and the bulk of the M band emission originates farther away than a few hundred parsec, was tested. The idea was to look for evidence of absorption of the diffuse background radiation by nearby interstellar clouds.

XAS Studies of Arsenic in the Environment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Charnock, J. M.; School of Earth, Atmospheric and Environmental Sciences, University of Manchester, Oxford Road, Manchester, M13 9PL; Polya, D. A.

2007-02-02

Arsenic is present in low concentrations in much of the Earth's crust and changes in its speciation are vital to understanding its transport and toxicity in the environment. We have used X-ray absorption spectroscopy to investigate the coordination sites of arsenic in a wide variety of samples, including soil and earthworm tissues from arsenic-contaminated land, and human hair and nail samples from people exposed to arsenic in Cambodia. Our results confirm the effectiveness of using X-ray absorption near edge structure (XANES) and X-ray absorption fine structure (EXAFS) spectroscopy to determine speciation changes in environmental samples.

Role of relaxation and time-dependent formation of x-ray spectra

NASA Astrophysics Data System (ADS)

Privalov, Timofei; Gel'mukhanov, Faris; Ågren, Hans

2001-10-01

A fundamental problem of x-ray spectroscopy is the role of relaxation of the electronic subsystem in the field of the transient core hole. The main intention of the present study is to explore the dynamics due to core-hole relaxation in the whole time domain, and to find out how it is manifested in finite molecular systems in comparison with solids. A technique is developed based on a reduction of the Noziéres-De Dominicis equation to a set of linear algebraic equations. The developed time-dependent formalism is applied to a numerical investigation of a one-dimensional tight-binding model. The formation of the x-ray profiles is explored on the real time scale, and the role of interaction with the core hole, band filling, and the final-state rule are investigated for systems of different size. The formation of spectra of the infinite translational invariant system is studied by extensions of the finite systems. We found that the dynamics of finite systems, like molecules, differs qualitatively from solids: Contrary to the latter the time lapse of the Noziéres-De Dominicis domain for finite systems is squeezed between the inverse bandwidth and the revival time, which is proportional to the system size. For small molecules this means that there is no time for a ``Mahan-Noziéres-De Dominicis singularity'' to develop. Comparison with the strict solution of the Noziéres-De Dominicis equation shows that the adiabatic approximation describes x-ray absorption and emission considerably better than the fast approximation. This explains the suppression of the relaxation effects in x-ray emission of, e.g., gas phase and surface adsorbed molecules, but also that these effects are essential for the absorption case. There is still a quantitative distinction between the adiabatic approximation and the strict approach, which becomes more important for larger systems. Adopting the so-called finite state rule by von Barth and Grossman also for molecules, an almost complete numerical agreement between this rule and the strict x-ray-absorption and emission profiles for systems of different sizes is obtained. The simulations indicate that the final-state rule correction is important mainly near the absorption edge and at the top of the emission band.

Determination of low-Z elements in individual environmental particles using windowless EPMA.

PubMed

Ro, C U; Osán, J; Van Grieken, R

1999-04-15

The determination of low-Z elements such as carbon, nitrogen, and oxygen in atmospheric aerosol particles is of interest in studying environmental pollution. Conventional electron probe microanalysis technique has a limitation for the determination of the low-Z elements, mainly because the Be window in an energy-dispersive X-ray (EDX) detector hinders the detection of characteristic X-rays from light elements. The feasibility of low-Z element determination in individual particles using a windowless EDX detector is investigated. To develop a method capable of identifying chemical species of individual particles, both the matrix and the geometric effects of particles have to be evaluated. X-rays of low-Z elements generated by an electron beam are so soft that important matrix effects, mostly due to X-ray absorption, exist even within particles in the micrometer size range. Also, the observed radiation, especially that of light elements, experiences different extents of absorption, depending on the shape and size of the particles. Monte Carlo calculation is applied to explain the variation of observed X-ray intensities according to the geometric and chemical compositional variation of individual particles, at different primary electron beam energies. A comparison is carried out between simulated and experimental data, collected for standard individual particles with chemical compositions as generally observed in marine and continental aerosols. Despite the many fundamental problematic analytical factors involved in the observation of X-rays from low-Z elements, the Monte Carlo calculation proves to be quite reliable to evaluate those matrix and geometric effects. Practical aspects of the Monte Carlo calculation for the determination of light elements in individual particles are also considered.

Micro-x-ray fluorescence, micro-x-ray absorption spectroscopy, and micro-x-ray diffraction investigation of lead speciation after the addition of different phosphorus amendments to a smelter-contaminated soil.

PubMed

Baker, Lucas R; Pierzynski, Gary M; Hettiarachchi, Ganga M; Scheckel, Kirk G; Newville, Matthew

2014-03-01

The stabilization of Pb on additions of P to contaminated soils and mine spoil materials has been well documented. It is clear from the literature that different P sources result in different efficacies of Pb stabilization in the same contaminated material. We hypothesized that the differences in the efficacy of Pb stabilization in contaminated soils on fluid or granular P amendment addition is due to different P reaction processes in and around fertilizer granules and fluid droplets. We used a combination of several synchrotron-based techniques (i.e., spatially resolved micro-X-ray fluorescence, micro-X-ray absorption near-edge structure spectroscopy, and micro-X-ray diffraction) to speciate Pb at two incubation times in a smelter-contaminated soil on addition of several fluid and granular P amendments. The results indicated that the Pb phosphate mineral plumbogummite was an intermediate phase of pyromorphite formation. Additionally, all fluid and granular P sources were able to induce Pb phosphate formation, but fluid phosphoric acid (PA) was the most effective with time and distance from the treatment. Granular phosphate rock and triple super phosphate (TSP) amendments reacted to generate Pb phosphate minerals, with TSP being more effective at greater distances from the point of application. As a result, PA and TSP were the most effective P amendments at inducing Pb phosphate formation, but caution needs to be exercised when adding large amounts of soluble P to the environment. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

Equally sloped X-ray microtomography of living insects with low radiation dose and improved resolution capability

NASA Astrophysics Data System (ADS)

Yao, Shengkun; Fan, Jiadong; Zong, Yunbing; He, You; Zhou, Guangzhao; Sun, Zhibin; Zhang, Jianhua; Huang, Qingjie; Xiao, Tiqiao; Jiang, Huaidong

2016-03-01

Three-dimensional X-ray imaging of living specimens is challenging due to the limited resolution of conventional absorption contrast X-ray imaging and potential irradiation damage of biological specimens. In this letter, we present microtomography of a living specimen combining phase-contrast imaging and a Fourier-based iterative algorithm termed equally sloped tomography. Non-destructive 3D imaging of an anesthetized living yellow mealworm Tenebrio molitor was demonstrated with a relatively low dose using synchrotron generated X-rays. Based on the high-quality 3D images, branching tracheoles and different tissues of the insect in a natural state were identified and analyzed, demonstrating a significant advantage of the technique over conventional X-ray radiography or histotomy. Additionally, the insect survived without problem after a 1.92-s X-ray exposure and subsequent absorbed radiation dose of ˜1.2 Gy. No notable physiological effects were observed after reviving the insect from anesthesia. The improved static tomographic method demonstrated in this letter shows advantage in the non-destructive structural investigation of living insects in three dimensions due to the low radiation dose and high resolution capability, and offers many potential applications in biological science.

Equally sloped X-ray microtomography of living insects with low radiation dose and improved resolution capability

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yao, Shengkun; Fan, Jiadong; Zong, Yunbing

Three-dimensional X-ray imaging of living specimens is challenging due to the limited resolution of conventional absorption contrast X-ray imaging and potential irradiation damage of biological specimens. In this letter, we present microtomography of a living specimen combining phase-contrast imaging and a Fourier-based iterative algorithm termed equally sloped tomography. Non-destructive 3D imaging of an anesthetized living yellow mealworm Tenebrio molitor was demonstrated with a relatively low dose using synchrotron generated X-rays. Based on the high-quality 3D images, branching tracheoles and different tissues of the insect in a natural state were identified and analyzed, demonstrating a significant advantage of the technique overmore » conventional X-ray radiography or histotomy. Additionally, the insect survived without problem after a 1.92-s X-ray exposure and subsequent absorbed radiation dose of ∼1.2 Gy. No notable physiological effects were observed after reviving the insect from anesthesia. The improved static tomographic method demonstrated in this letter shows advantage in the non-destructive structural investigation of living insects in three dimensions due to the low radiation dose and high resolution capability, and offers many potential applications in biological science.« less

Microfabrication of High Resolution X-ray Magnetic Calorimeters

NASA Astrophysics Data System (ADS)

Hsieh, Wen-Ting; Bandler, Simon R.; Kelly, Daniel P.; Porst, Jan P.; Rotzinger, Hannes; Seidel, George M.; Stevenson, Thomas R.

2009-12-01

Metallic magnetic calorimeter (MMC) is one of the most promising x-ray detector technologies for providing the very high energy resolution needed for future astronomical x-ray imaging spectroscopy. For this purpose, we have developed micro-fabricated 5×5 arrays of MMC of which each individual pixel has excellent energy resolution as good as 3.4 eV at 6 keV x-ray. Here we report on the fabrication techniques developed to achieve good resolution and high efficiency. These include: processing of a thin insulation layer for strong magnetic coupling between the AuEr sensor film and the niobium pick-up coil; production of overhanging absorbers for enhanced efficiency of x-ray absorption; fabrication on SiN membranes to minimize the effects on energy resolution from athermal phonon loss. We have also improved the deposition of the magnetic sensor film such that the film magnetization is nearly completely that is expected from the AuEr sputter target bulk material. In addition, we have included a study of a positional sensitive design, the Hydra design, which allows thermal coupling of four absorbers to a common MMC sensor and circuit.

Weak Hard X-Ray Emission from Two Broad Absorption Line Quasars Observed with NuStar: Compton-Thick Absorption or Intrinsic X-Ray Weakness?

NASA Technical Reports Server (NTRS)

Luo, B.; Brandt, W. N.; Alexander, D. M.; Harrison, F. A.; Stern, D.; Bauer, F. E.; Boggs, S. E.; Christensen, F. E.; Comastri, A.; Craig, W. W..;

WEAK HARD X-RAY EMISSION FROM TWO BROAD ABSORPTION LINE QUASARS OBSERVED WITH NuSTAR: COMPTON-THICK ABSORPTION OR INTRINSIC X-RAY WEAKNESS?

DOE Office of Scientific and Technical Information (OSTI.GOV)

Luo, B.; Brandt, W. N.; Alexander, D. M.

We present Nuclear Spectroscopic Telescope Array (NuSTAR) hard X-ray observations of two X-ray weak broad absorption line (BAL) quasars, PG 1004+130 (radio loud) and PG 1700+518 (radio quiet). Many BAL quasars appear X-ray weak, probably due to absorption by the shielding gas between the nucleus and the accretion-disk wind. The two targets are among the optically brightest BAL quasars, yet they are known to be significantly X-ray weak at rest-frame 2-10 keV (16-120 times fainter than typical quasars). We would expect to obtain Almost-Equal-To 400-600 hard X-ray ({approx}> 10 keV) photons with NuSTAR, provided that these photons are not significantlymore » absorbed (N{sub H} {approx}< 10{sup 24} cm{sup -2}). However, both BAL quasars are only detected in the softer NuSTAR bands (e.g., 4-20 keV) but not in its harder bands (e.g., 20-30 keV), suggesting that either the shielding gas is highly Compton-thick or the two targets are intrinsically X-ray weak. We constrain the column densities for both to be N{sub H} Almost-Equal-To 7 Multiplication-Sign 10{sup 24} cm{sup -2} if the weak hard X-ray emission is caused by obscuration from the shielding gas. We discuss a few possibilities for how PG 1004+130 could have Compton-thick shielding gas without strong Fe K{alpha} line emission; dilution from jet-linked X-ray emission is one likely explanation. We also discuss the intrinsic X-ray weakness scenario based on a coronal-quenching model relevant to the shielding gas and disk wind of BAL quasars. Motivated by our NuSTAR results, we perform a Chandra stacking analysis with the Large Bright Quasar Survey BAL quasar sample and place statistical constraints upon the fraction of intrinsically X-ray weak BAL quasars; this fraction is likely 17%-40%.« less

High Resolution X-Ray Absorption Spectroscopy: Distribution of Matter in and around Galaxies

NASA Astrophysics Data System (ADS)

Schulz, Norbert; MIT/CAT Team

2015-10-01

The chemical evolution of the Universe embraces aspects that reachdeep into modern astrophysics and cosmology. We want to know how present and past matter is affected by various levels and types of nucleo-synthesis and stellar evolution. Three major categories were be identified: 1. The study of pre-mordial star formation including periods of super-massive black hole formation, 2. The embedded evolution of the intergalactic medium IGM, 3. The status and evolution of stars and the interstellar medium ISM in galaxies. Today a fourth category relates to our understanding of dark matter in relationwith these three categories. The X-ray band is particularly sensitive to K- and L-shell absorption and scattering from high abundant elements like C, N, O, Ne, Mg, Si, S,Ar, Ca, Fe, and Ni. Like the Lyman alpha forest in the optical band, absorbers in the IGM produce an X-ray line forest along the line of sight in the X-rayspectrum of a background quasar. Similary bright X-ray sources within galaxies and the Milky Way produce a continuum, which is being absorbed by elements invarious phases of the ISM. High resolution X-ray absorption surveys are possible with technologies ready for flight within decade. == high efficiency X-ray optics with optical performance 3== high resolution X-ray gratings with R 3000 for E 1.5 keV== X-ray micro-calorimeters with R 2000 for E 1.5 keV. The vision for the next decade needs to lead to means and strategies which allows us to perform such absorption surveys as effectively as surveys are now or in very near future quite common in astronomy pursued in other wave length bands such as optical, IR, and sub-mm.

Quasar Absorption Studies

NASA Technical Reports Server (NTRS)

Mushotzky, Richard (Technical Monitor); Elvis, Martin

2004-01-01

The aim of the proposal is to investigate the absorption properties of a sample of inter-mediate redshift quasars. The main goals of the project are: Measure the redshift and the column density of the X-ray absorbers; test the correlation between absorption and redshift suggested by ROSAT and ASCA data; constrain the absorber ionization status and metallicity; constrain the absorber dust content and composition through the comparison between the amount of X-ray absorption and optical dust extinction. Unanticipated low energy cut-offs where discovered in ROSAT spectra of quasars and confirmed by ASCA, BeppoSAX and Chandra. In most cases it was not possible to constrain adequately the redshift of the absorber from the X-ray data alone. Two possibilities remain open: a) absorption at the quasar redshift; and b) intervening absorption. The evidences in favour of intrinsic absorption are all indirect. Sensitive XMM observations can discriminate between these different scenarios. If the absorption is at the quasar redshift we can study whether the quasar environment evolves with the Cosmic time.

Unveiling the X-ray/UV properties of AGN winds using Broad and mini-Broad Absorption Line Quasars

NASA Astrophysics Data System (ADS)

Giustini, M.

2015-07-01

BAL/mini-BALs are observed in the UV spectra of ˜ 20-30% of optically selected AGN as broad absorption troughs blueshifted by several thousands km/s, indicative of powerful nuclear winds. They could be representative of the average AGN if their winds cover only 20-30% of the continuum source, and/or represent an evolutionary state analogous to the high-soft state of BHB, when the jet emission is quenched and strong X-ray absorbing equatorial disk winds are virtually ubiquitous. High-quality, possibly time-resolved X-ray/UV studies are crucial to assess the global amount and 'character' of absorption in BAL/mini-BAL QSOs and to constrain the physical mechanism responsible for the launch and acceleration of their winds, therefore placing them in the broader context of AGN geometry and evolution. I will review here the known X-ray properties of BAL/mini-BAL QSOs, and present new results from a comprehensive X-ray spectral analysis of all the Palomar-Green BAL/mini-BAL QSOs with available XMM-Newton observations, for a total of 51 pointings of 14 different sources. These will include the most recent results from a high-quality simultaneous XMM/HST observational campaign on the mini-BAL QSO PG 1126-041, that unveiled with stunning details the X-ray/UV connection in action in an AGN disk wind through correlated X-ray/UV absorption variability.

Tuning the nonlinear optical absorption in Au/BaTiO3 nanocomposites with gold nanoparticle concentration

NASA Astrophysics Data System (ADS)

Bijeesh, M. M.; Shakhi, P. K.; Varier, Geetha K.; Nandakumar, P.

2018-06-01

We report on the nonlinear optical absorption coefficient of Au/BaTiO3 nanocomposite films and its dependence on gold nanoparticle concentration. Au/BaTiO3 nanocomposite films with different molar ratio of Au/Ba are prepared by sol-gel technique and characterized by X-ray diffraction, UV Visible absorption spectroscopy and high resolution transmission electron microscopy. An open aperture Z-scan technique is employed to study the third order nonlinear optical properties of Au/BaTiO3 thin films. An Nd:YAG laser operating at 532 nm wavelength having a pulse width of 5 ns is used for the measurements. The two-photon absorption coefficient of the films increases linearly with gold nanoparticle concentration and significant enhancement of nonlinear optical absorption is observed. This ability to fine tune the nonlinear optical coefficients of Au/BaTiO3 films would be handy in optical device applications.

Comparative Analysis of Microbial Communities in Iron-Dominated Flocculent Mats in Deep-Sea Hydrothermal Environments.

PubMed

Makita, Hiroko; Kikuchi, Sakiko; Mitsunobu, Satoshi; Takaki, Yoshihiro; Yamanaka, Toshiro; Toki, Tomohiro; Noguchi, Takuroh; Nakamura, Kentaro; Abe, Mariko; Hirai, Miho; Yamamoto, Masahiro; Uematsu, Katsuyuki; Miyazaki, Junichi; Nunoura, Takuro; Takahashi, Yoshio; Takai, Ken

2016-10-01

It has been suggested that iron is one of the most important energy sources for photosynthesis-independent microbial ecosystems in the ocean crust. Iron-metabolizing chemolithoautotrophs play a key role as primary producers, but little is known about their distribution and diversity and their ecological role as submarine iron-metabolizing chemolithotrophs, particularly the iron oxidizers. In this study, we investigated the microbial communities in several iron-dominated flocculent mats found in deep-sea hydrothermal fields in the Mariana Volcanic Arc and Trough and the Okinawa Trough by culture-independent molecular techniques and X-ray mineralogical analyses. The abundance and composition of the 16S rRNA gene phylotypes demonstrated the ubiquity of zetaproteobacterial phylotypes in iron-dominated mat communities affected by hydrothermal fluid input. Electron microscopy with energy-dispersive X-ray microanalysis and X-ray absorption fine structure (XAFS) analysis revealed the chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species and the potential contribution of Zetaproteobacteria to the in situ generation. These results suggest that putative iron-oxidizing chemolithoautotrophs play a significant ecological role in producing iron-dominated flocculent mats and that they are important for iron and carbon cycles in deep-sea low-temperature hydrothermal environments. We report novel aspects of microbiology from iron-dominated flocculent mats in various deep-sea environments. In this study, we examined the relationship between Zetaproteobacteria and iron oxides across several hydrothermally influenced sites in the deep sea. We analyzed iron-dominated mats using culture-independent molecular techniques and X-ray mineralogical analyses. The scanning electron microscopy-energy-dispersive X-ray spectroscopy SEM-EDS analysis and X-ray absorption fine structure (XAFS) analysis revealed chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species as well as the potential contribution of the zetaproteobacterial population to the in situ production. These key findings provide important information for understanding the mechanisms of both geomicrobiological iron cycling and the formation of iron-dominated mats in deep-sea hydrothermal fields. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

Ultrathin Limit of Exchange Bias Coupling at Oxide Multiferroic/Ferromagnetic Interfaces

DTIC Science & Technology

2013-07-12

perfect, lattice-matched hetero- structures of complex perovskite oxides using state-of-the-art thin fi lm growth techniques has generated new physical...investigated for several BFO/LSMO heterostructures by X-ray absorption spectroscopy (XAS) measurements at 17 K of the Fe- L 2,3 edge at the Advanced Light

Performance of a Zerovalent Iron Reactive Barrier for the Treatment of Arsenic in Groundwater: Part 2. Geochemical Modeling and Solid Phase Studies

EPA Science Inventory

Arsenic uptake processes were evaluated in a zerovalent iron reactive barrier installed at a lead smelting facility using geochemical modeling, solid-phase analysis, and X-ray absorption spectroscopy techniques. Aqueous speciation of arsenic plays a key role in directing arsenic...

Telescope for x ray and gamma ray studies in astrophysics

NASA Technical Reports Server (NTRS)

Weaver, W. D.; Desai, Upendra D.

1993-01-01

Imaging of x-rays has been achieved by various methods in astrophysics, nuclear physics, medicine, and material science. A new method for imaging x-ray and gamma-ray sources avoids the limitations of previously used imaging devices. Images are formed in optical wavelengths by using mirrors or lenses to reflect and refract the incoming photons. High energy x-ray and gamma-ray photons cannot be reflected except at grazing angles and pass through lenses without being refracted. Therefore, different methods must be used to image x-ray and gamma-ray sources. Techniques using total absorption, or shadow casting, can provide images in x-rays and gamma-rays. This new method uses a coder made of a pair of Fresnel zone plates and a detector consisting of a matrix of CsI scintillators and photodiodes. The Fresnel zone plates produce Moire patterns when illuminated by an off-axis source. These Moire patterns are deconvolved using a stepped sine wave fitting or an inverse Fourier transform. This type of coder provides the capability of an instantaneous image with sub-arcminute resolution while using a detector with only a coarse position-sensitivity. A matrix of the CsI/photodiode detector elements provides the necessary coarse position-sensitivity. The CsI/photodiode detector also allows good energy resolution. This imaging system provides advantages over previously used imaging devices in both performance and efficiency.

Spectral studies of cosmic X-ray sources

NASA Astrophysics Data System (ADS)

Blissett, R. J.

1980-01-01

The conventional "indirect" method of reduction and data analysis of spectral data from non-dispersive X-ray detectors, by the fitting of assumed spectral models, is examined. The limitations of this procedure are presented, and alternative schemes are considered in which the derived spectra are not biased to an astrophysical source model. A new method is developed in detail to directly restore incident photon spectra from the detected count histograms. This Spectral Restoration Technique allows an increase in resolution, to a degree dependent on the statistical precision of the data. This is illustrated by numerical simulations. Proportional counter data from Ariel 5 are analysed using this technique. The results obtained for the sources Cas A and the Crab Nebula are consistent with previous analyses and show that increases in resolution of up to a factor three are possible in practice. The source Cyg X-3 is closely examined. Complex spectral variability is found, with the continuum and iron-line emission modulated with the 4.8 hour period of the source. The data suggest multi-component emission in the source. Comparing separate Ariel 5 observations and published data from other experiments, a correlation between the spectral shape and source intensity is evident. The source behaviour is discussed with reference to proposed source models. Data acquired by the low-energy detectors on-board HEAO-1 are analysed using the Spectral Restoration Technique. This treatment explicitly demonstrates the existence of oxygen K-absorption edges in the soft X-ray spectra of the Crab Nebula and Sco X-1. These results are considered with reference to current theories of the interstellar medium. The thesis commences with a review of cosmic X-ray sources and the mechanisms responsible for their spectral signatures, and continues with a discussion of the instruments appropriate for spectral studies in X-ray astronomy.

X-ray absorption microtomography (microCT) and small beam diffraction mapping of sea urchin teeth.

PubMed

Stock, S R; Barss, J; Dahl, T; Veis, A; Almer, J D

2002-07-01

Two noninvasive X-ray techniques, laboratory X-ray absorption microtomography (microCT) and X-ray diffraction mapping, were used to study teeth of the sea urchin Lytechinus variegatus. MicroCT revealed low attenuation regions at near the tooth's stone part and along the carinar process-central prism boundary; this latter observation appears to be novel. The expected variation of Mg fraction x in the mineral phase (calcite, Ca(1-x)Mg(x)CO(3)) cannot account for all of the linear attenuation coefficient decrease in the two zones: this suggested that soft tissue is localized there. Transmission diffraction mapping (synchrotron X-radiation, 80.8 keV, 0.1 x 0.1mm(2) beam area, 0.1mm translation grid, image plate area detector) simultaneously probed variations in 3-D and showed that the crystal elements of the "T"-shaped tooth were very highly aligned. Diffraction patterns from the keel (adaxial web) and from the abaxial flange (containing primary plates and the stone part) differed markedly. The flange contained two populations of identically oriented crystal elements with lattice parameters corresponding to x=0.13 and x=0.32. The keel produced one set of diffraction spots corresponding to the lower x. The compositions were more or less equivalent to those determined by others for camarodont teeth, and the high Mg phase is expected to be disks of secondary mineral epitaxially related to the underlying primary mineral element. Lattice parameter gradients were not noted in the keel or flange. Taken together, the microCT and diffraction results indicated that there was a band of relatively high protein content, of up to approximately 0.25 volume fraction, in the central part of the flange and paralleling its adaxial and abaxial faces. X-ray microCT and microdiffraction data used in conjunction with protein distribution data will be crucial for understanding the properties of various biocomposites and their mechanical functions.

Transport Measurements and Synchrotron-Based X-Ray Absorption Spectroscopy of Iron Silicon Germanide Grown by Molecular Beam Epitaxy

NASA Astrophysics Data System (ADS)

Elmarhoumi, Nader; Cottier, Ryan; Merchan, Greg; Roy, Amitava; Lohn, Chris; Geisler, Heike; Ventrice, Carl, Jr.; Golding, Terry

2009-03-01

Some of the iron-based metal silicide and germanide phases have been predicted to be direct band gap semiconductors. Therefore, they show promise for use as optoelectronic materials. We have used synchrotron-based x-ray absorption spectroscopy to study the structure of iron silicon germanide films grown by molecular beam epitaxy. A series of Fe(Si1-xGex)2 thin films (2000 -- 8000å) with a nominal Ge concentration of up to x = 0.04 have been grown. X-ray absorption near edge structure (XANES) and extended x-ray absorption fine structure (EXAFS) measurements have been performed on the films. The nearest neighbor co-ordination corresponding to the β-FeSi2 phase of iron silicide provides the best fit with the EXAFS data. Temperature dependent (20 < T < 350 K) magneto transport measurements were done on the Fe(Si1-xGex)2 thin films via Van Der Paw (VDP) Hall configuration using a 0.5-1T magnetic field and a current of 10-200 μA through indium ohmic contacts, the Hall coefficient was calculated. Results suggest semiconducting behavior of the films which is consistent with the EXAFS results.

Phase contrast imaging with coherent high energy X-rays

DOE Office of Scientific and Technical Information (OSTI.GOV)

Snigireva, I.

X-ray imaging concern high energy domain (>6 keV) like a contact radiography, projection microscopy and tomography is used for many years to discern the features of the internal structure non destructively in material science, medicine and biology. In so doing the main contrast formation is absorption that makes some limitations for imaging of the light density materials and what is more the resolution of these techniques is not better than 10-100 {mu}m. It was turned out that there is now way in which to overcome 1{mu}m or even sub-{mu}m resolution limit except phase contrast imaging. It is well known inmore » optics that the phase contrast is realised when interference between reference wave front and transmitted through the sample take place. Examples of this imaging are: phase contrast microscopy suggested by Zernike and Gabor (in-line) holography. Both of this techniques: phase contrast x-ray microscopy and holography are successfully progressing now in soft x-ray region. For imaging in the hard X-rays to enhance the contrast and to be able to resolve phase variations across the beam the high degree of the time and more importantly spatial coherence is needed. Because of this it was reasonable that the perfect crystal optics was involved like Bonse-Hart interferometry, double-crystal and even triple-crystal set-up using Laue and Bragg geometry with asymmetrically cut crystals.« less

Multispecies Biofilms Transform Selenium Oxyanions into Elemental Selenium Particles: Studies Using Combined Synchrotron X-ray Fluorescence Imaging and Scanning Transmission X-ray Microscopy.

PubMed

Yang, Soo In; George, Graham N; Lawrence, John R; Kaminskyj, Susan G W; Dynes, James J; Lai, Barry; Pickering, Ingrid J

2016-10-04

Selenium (Se) is an element of growing environmental concern, because low aqueous concentrations can lead to biomagnification through the aquatic food web. Biofilms, naturally occurring microbial consortia, play numerous important roles in the environment, especially in biogeochemical cycling of toxic elements in aquatic systems. The complexity of naturally forming multispecies biofilms presents challenges for characterization because conventional microscopic techniques require chemical and physical modifications of the sample. Here, multispecies biofilms biotransforming selenium oxyanions were characterized using X-ray fluorescence imaging (XFI) and scanning transmission X-ray microscopy (STXM). These complementary synchrotron techniques required minimal sample preparation and were applied correlatively to the same biofilm areas. Sub-micrometer XFI showed distributions of Se and endogenous metals, while Se K-edge X-ray absorption spectroscopy indicated the presence of elemental Se (Se 0 ). Nanoscale carbon K-edge STXM revealed the distributions of microbial cells, extracellular polymeric substances (EPS), and lipids using the protein, saccharide, and lipid signatures, respectively, together with highly localized Se 0 using the Se L III edge. Transmission electron microscopy showed the electron-dense particle diameter to be 50-700 nm, suggesting Se 0 nanoparticles. The intimate association of Se 0 particles with protein and polysaccharide biofilm components has implications for the bioavailability of selenium in the environment.

Multispecies Biofilms Transform Selenium Oxyanions into Elemental Selenium Particles: Studies Using Combined Synchrotron X-ray Fluorescence Imaging and Scanning Transmission X-ray Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Soo In; George, Graham N.; Lawrence, John R.

2016-10-04

Selenium (Se) is an element of growing environmental concern, because low aqueous concentrations can lead to biomagnification through the aquatic food web. Biofilms, naturally occurring microbial consortia, play numerous important roles in the environment, especially in biogeochemical cycling of toxic elements in aquatic systems. The complexity of naturally forming multispecies biofilms presents challenges for characterization because conventional microscopic techniques require chemical and physical modifications of the sample. Here, multispecies biofilms biotransforming selenium oxyanions were characterized using X-ray fluorescence imaging (XFI) and scanning transmission X-ray microscopy (STXM). These complementary synchrotron techniques required minimal sample preparation and were applied correlatively to themore » same biofilm areas. Sub-micrometer XFI showed distributions of Se and endogenous metals, while Se K-edge X-ray absorption spectroscopy indicated the presence of elemental Se (Se0). Nanoscale carbon K-edge STXM revealed the distributions of microbial cells, extracellular polymeric substances (EPS), and lipids using the protein, saccharide, and lipid signatures, respectively, together with highly localized Se0 using the Se LIII edge. Transmission electron microscopy showed the electron-dense particle diameter to be 50–700 nm, suggesting Se0 nanoparticles. The intimate association of Se0 particles with protein and polysaccharide biofilm components has implications for the bioavailability of selenium in the environment.« less

Magnetic nanoparticles formed in glasses co-doped with iron and larger radius elements

NASA Astrophysics Data System (ADS)

Edelman, I.; Ivanova, O.; Ivantsov, R.; Velikanov, D.; Zabluda, V.; Zubavichus, Y.; Veligzhanin, A.; Zaikovskiy, V.; Stepanov, S.; Artemenko, A.; Curély, J.; Kliava, J.

2012-10-01

A new type of nanoparticle-containing glasses based on borate glasses co-doped with low contents of iron and larger radius elements, Dy, Tb, Gd, Ho, Er, Y, and Bi, is studied. Heat treatment of these glasses results in formation of magnetic nanoparticles, radically changing their physical properties. Transmission electron microscopy and synchrotron radiation-based techniques: x-ray diffraction, extended x-ray absorption fine structure, x-ray absorption near-edge structure, and small-angle x-ray scattering, show a broad distribution of nanoparticle sizes with characteristics depending on the treatment regime; a crystalline structure of these nanoparticles is detected in heat treated samples. Magnetic circular dichroism (MCD) studies of samples subjected to heat treatment as well as of maghemite, magnetite, and iron garnet allow to unambiguously assign the nanoparticle structure to maghemite, independently of co-dopant nature and of heat treatment regime used. Different features observed in the MCD spectra are related to different electron transitions in Fe3+ ions gathered in the nanoparticles. The static magnetization in heat treated samples has non-linear dependence on the magnetizing field with hysteresis. Zero-field cooled magnetization curves show that at higher temperatures the nanoparticles occur in superparamagnetic state with blocking temperatures above 100 K. Below ca. 20 K, a considerable contribution to both zero field-cooled and field-cooled magnetizations occurs from diluted paramagnetic ions. Variable-temperature electron magnetic resonance (EMR) studies unambiguously show that in as-prepared glasses paramagnetic ions are in diluted state and confirm the formation of magnetic nanoparticles already at earlier stages of heat treatment. Computer simulations of the EMR spectra corroborate the broad distribution of nanoparticle sizes found by "direct" techniques as well as superparamagnetic nanoparticle behaviour demonstrated in the magnetization studies.

Time-dependent nonequilibrium soft x-ray response during a spin crossover

DOE Office of Scientific and Technical Information (OSTI.GOV)

van Veenendaal, Michel

The rapid development of high-brilliance pulsed X-ray sources with femtosecond time resolution has created a need for a better theoretical understanding of the time-dependent soft-X-ray response of dissipative many-body quantum systems. It is demonstrated how soft-X-ray spectroscopies, such as X-ray absorption and resonant inelastic X-ray scattering at transition-metal L-edges, can provide insight into intersystem crossings, such as a spin crossover. The photoinduced doublet-to-quartet spin crossover on cobalt in Fe-Co Prussian blue analogues is used as an example to demonstrate how the X-ray response is affected by the dissipative nonequilibrium dynamics. The time-dependent soft-X-ray spectra provide a wealth of information thatmore » reflect the changes in the nonequilibrium initial state via continuously changing spectral lineshapes that cannot be decomposed into initial photoexcited and final metastable spectra, strong broadenings, a collapse of clear selection rules during the intersystem crossing, strong fluctuations in the isotropic branching ratio in X-ray absorption, and crystal-field collapse/oscillations and strongly time-dependent anti-Stokes processes in RIXS.« less

High Resolution X-ray-Induced Acoustic Tomography

PubMed Central

Xiang, Liangzhong; Tang, Shanshan; Ahmad, Moiz; Xing, Lei

2016-01-01

Absorption based CT imaging has been an invaluable tool in medical diagnosis, biology, and materials science. However, CT requires a large set of projection data and high radiation dose to achieve superior image quality. In this letter, we report a new imaging modality, X-ray Induced Acoustic Tomography (XACT), which takes advantages of high sensitivity to X-ray absorption and high ultrasonic resolution in a single modality. A single projection X-ray exposure is sufficient to generate acoustic signals in 3D space because the X-ray generated acoustic waves are of a spherical nature and propagate in all directions from their point of generation. We demonstrate the successful reconstruction of gold fiducial markers with a spatial resolution of about 350 μm. XACT reveals a new imaging mechanism and provides uncharted opportunities for structural determination with X-ray. PMID:27189746

Design, Fabrication and Testing of Multilayer Coated X-Ray Optics for the Water Window Imaging X-Ray Microscope

NASA Technical Reports Server (NTRS)

Spencer, Dwight C.

1996-01-01

Hoover et. al. built and tested two imaging Schwarzschild multilayer microscopes. These instruments were constructed as prototypes for the "Water Window Imaging X-Ray Microscope," which is a doubly reflecting, multilayer x-ray microscope configured to operate within the "water window." The "water window" is the narrow region of the x-ray spectrum between the K absorption edges of oxygen (lamda = 23.3 Angstroms) and of carbon (lamda = 43.62 Angstroms), where water is relatively highly transmissive and carbon is highly absorptive. This property of these materials, thus permits the use of high resolution multilayer x-ray microscopes for producing high contrast images of carbon-based structures within the aqueous physiological environments of living cells. We report the design, fabrication and testing of multilayer optics that operate in this regime.

Femtosecond time-resolved X-ray absorption spectroscopy of anatase TiO2 nanoparticles using XFEL

PubMed Central

Obara, Yuki; Ito, Hironori; Ito, Terumasa; Kurahashi, Naoya; Thürmer, Stephan; Tanaka, Hiroki; Katayama, Tetsuo; Togashi, Tadashi; Owada, Shigeki; Yamamoto, Yo-ichi; Karashima, Shutaro; Nishitani, Junichi; Yabashi, Makina; Suzuki, Toshinori; Misawa, Kazuhiko

2017-01-01

The charge-carrier dynamics of anatase TiO2 nanoparticles in an aqueous solution were studied by femtosecond time-resolved X-ray absorption spectroscopy using an X-ray free electron laser in combination with a synchronized ultraviolet femtosecond laser (268 nm). Using an arrival time monitor for the X-ray pulses, we obtained a temporal resolution of 170 fs. The transient X-ray absorption spectra revealed an ultrafast Ti K-edge shift and a subsequent growth of a pre-edge structure. The edge shift occurred in ca. 100 fs and is ascribed to reduction of Ti by localization of generated conduction band electrons into shallow traps of self-trapped polarons or deep traps at penta-coordinate Ti sites. Growth of the pre-edge feature and reduction of the above-edge peak intensity occur with similar time constants of 300–400 fs, which we assign to the structural distortion dynamics near the surface. PMID:28713842

Probing the CZTS/CdS heterojunction utilizing photoelectrochemistry and x-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Turnbull, Matthew J.; Vaccarello, Daniel; Wong, Jonathan; Yiu, Yun Mui; Sham, Tsun-Kong; Ding, Zhifeng

2018-04-01

The importance of renewable resources is becoming more and more influential on research due to the depletion of fossil fuels. Cost-effective ways of harvesting solar energy should also be at the forefront of these investigations. Cu2ZnSnS4 (CZTS) solar cells are well within the frame of these goals, and a thorough understanding of how they are made and processed synthetically is crucial. The CZTS/CdS heterojunction was examined using photoelectrochemistry and synchrotron radiation (SR) spectroscopy. These tools provided physical insights into this interface that was formed by the electrophoretic deposition of CZTS nanocrystals and chemical bath deposition (CBD) of CdS for the respective films. It was discovered that CBD induced a change in the local and long range environment of the Zn in the CZTS lattice, which was detrimental to the photoresponse. X-ray absorption near-edge structures and extended X-ray absorption fine structures (EXAFSs) of the junction showed that this change was at an atomic level and was associated with the coordination of oxygen to zinc. This was confirmed through FEFF fitting of the EXAFS and through IR spectroscopy. It was found that this change in both photoresponse and the Zn coordination can be reversed with the use of low temperature annealing. Investigating CZTS through SR techniques provides detailed structural information of minor changes from the zinc perspective.

Detailed transient heme structures of Mb-CO in solution after CO dissociation: an X-ray transient absorption spectroscopic study.

PubMed

Stickrath, Andrew B; Mara, Michael W; Lockard, Jenny V; Harpham, Michael R; Huang, Jier; Zhang, Xiaoyi; Attenkofer, Klaus; Chen, Lin X

2013-04-25

Although understanding the structural dynamics associated with ligand photodissociation is necessary in order to correlate structure and function in biological systems, few techniques are capable of measuring the ultrafast dynamics of these systems in solution-phase at room temperature. We present here a detailed X-ray transient absorption (XTA) study of the photodissociation of CO-bound myoglobin (Fe(II)CO-Mb) in room-temperature aqueous buffer solution with a time resolution of 80 ps, along with a general procedure for handling biological samples under the harsh experimental conditions that transient X-ray experiments entail. The XTA spectra of (Fe(II)CO-Mb) exhibit significant XANES and XAFS alterations following 527 nm excitation, which remain unchanged for >47 μs. These spectral changes indicate loss of the CO ligand, resulting in a five-coordinate, domed heme, and significant energetic reorganization of the 3d orbitals of the Fe center. With the current experimental setup, each X-ray pulse in the pulse train, separated by ~153 ns, can be separately discriminated, yielding snapshots of the myoglobin evolution over time. These methods can be easily applied to other biological systems, allowing for simultaneous structural and electronic measurements of any biological system with both ultrafast and slow time resolutions, effectively mapping out all of the samples' relevant physiological processes.

Complex polarization propagator approach in the restricted open-shell, self-consistent field approximation: the near K-edge X-ray absorption fine structure spectra of allyl and copper phthalocyanine.

PubMed

Linares, Mathieu; Stafström, Sven; Rinkevicius, Zilvinas; Ågren, Hans; Norman, Patrick

2011-05-12

A presentation of the complex polarization propagator in the restricted open-shell self-consistent field approximation is given. It rests on a formulation of a resonant-convergent, first-order polarization propagator approach that makes it possible to directly calculate the X-ray absorption cross section at a particular frequency without explicitly addressing the excited states. The quality of the predicted X-ray spectra relates only to the type of density functional applied without any separate treatment of dynamical relaxation effects. The method is applied to the calculation of the near K-edge X-ray absorption fine structure spectra of allyl and copper phthalocyanine. Comparison is made between the spectra of the radicals and those of the corresponding cations and anions to assess the effect of the increase of electron charge in the frontier orbital. The method offers the possibility for unique assignment of symmetry-independent atoms. The overall excellent spectral agreement motivates the application of the method as a routine precise tool for analyzing X-ray absorption of large systems of technological interest.

X-ray Absorption Spectroscopy Characterization of a Li/S Cell

PubMed Central

Ye, Yifan; Kawase, Ayako; Song, Min-Kyu; Feng, Bingmei; Liu, Yi-Sheng; Marcus, Matthew A.; Feng, Jun; Cairns, Elton J.; Guo, Jinghua; Zhu, Junfa

2016-01-01

The X-ray absorption spectroscopy technique has been applied to study different stages of the lithium/sulfur (Li/S) cell life cycle. We have investigated how speciation of S in Li/S cathodes changes upon the introduction of CTAB (cetyltrimethylammonium bromide, CH3(CH2)15N+(CH3)3Br−) and with charge/discharge cycling. The introduction of CTAB changes the synthesis reaction pathway dramatically due to the interaction of CTAB with the terminal S atoms of the polysulfide ions in the Na2Sx solution. For the cycled Li/S cell, the loss of electrochemically active sulfur and the accumulation of a compact blocking insulating layer of unexpected sulfur reaction products on the cathode surface during the charge/discharge processes make the capacity decay. A modified coin cell and a vacuum-compatible three-electrode electro-chemical cell have been introduced for further in-situ/in-operando studies. PMID:28344271

Operando characterization of batteries using x-ray absorption spectroscopy: advances at the beamline XAFS at synchrotron Elettra

NASA Astrophysics Data System (ADS)

Aquilanti, Giuliana; Giorgetti, Marco; Dominko, Robert; Stievano, Lorenzo; Arčon, Iztok; Novello, Nicola; Olivi, Luca

2017-02-01

X-ray absorption spectroscopy is a synchrotron radiation based technique that is able to provide information on both local structure and electronic properties in a chemically selective manner. It can be used to characterize the dynamic processes that govern the electrochemical energy storage in batteries, and to shed light on the redox chemistry and changes in structure during galvanostatic cycling to design cathode materials with improved properties. Operando XAS studies have been performed at beamline XAFS at Elettra on different systems. For Li-ion batteries, a multiedge approach revealed the role of the different cathode components during the charge and discharge of the battery. In addition, Li-S batteries for automotive applications were studied. Operando sulfur K-edge XANES and EXAFS analysis was used to characterize the redox chemistry of sulfur, and to relate the electrochemical mechanism to its local structure.

Stabilization and enhanced energy gap by Mg doping in ɛ-phase Ga2O3 thin films

NASA Astrophysics Data System (ADS)

Bi, Xiaoyu; Wu, Zhenping; Huang, Yuanqi; Tang, Weihua

2018-02-01

Mg-doped Ga2O3 thin films with different doping concentrations were deposited on sapphire substrates using laser molecular beam epitaxy (L-MBE) technique. X-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS) and ultraviolet-visible (UV-vis) absorption spectrum were used to characterize the crystal structure and optical properties of the as-grown films. Compared to pure Ga2O3 thin film, the Mg-doped thin films have transformed from the most stable β-phase into ɛ-phase. The absorption edge shifted to about 205 nm and the optical bandgap increased to ˜ 6 eV. These properties reveal that Mg-doped Ga2O3 films may have potential applications in the field of deep ultraviolet optoelectronic devices, such as deep ultraviolet photodetectors, short wavelength light emitting devices and so on.

X-Ray Absorption near Edge Structure Spectroscopy of Nanodiamonds from the Allende Meteorite

NASA Technical Reports Server (NTRS)

Flynn, G. J.; Keller, L. P.; Hill, H.; Jacobsen, C.; Wirick, S.

2000-01-01

Carbon X-ray Absorption Near Edge Structure Spectroscopy shows Allende DM nanodiamonds have two pre-edge peaks, consistent with other small diamonds, but fail to show a diamond exciton which is seen in 3.6 nm diamond thin films.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wojciech, Blachucki

This work treats of the high energy resolution off-resonant X-ray spectroscopy (HEROS) method of determining the density of unoccupied electronic states in the vicinity of the absorption edge. HEROS is an alternative to the existing X-ray absorption spectroscopy (XAS) methods and opens the way for new studies not achievable before.

Extended x-ray absorption fine structure spectroscopy and x-ray absorption near edge spectroscopy study of aliovalent doped ceria to correlate local structural changes with oxygen vacancies clustering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shirbhate, S. C.; Acharya, S. A., E-mail: saha275@yahoo.com; Yadav, A. K.

2016-04-04

This study provides atomic scale insight to understand the role of aliovalent dopants on oxygen vacancies clustering and dissociation mechanism in ceria system in order to enhance the performance of oxy-ion conductor. Dopants induced microscale changes in ceria are probed by extended X-ray absorption fine structure spectroscopy, X-ray absorption near edge spectra, and Raman spectroscopy. The results are explored to establish a correlation between atomic level structural changes (coordination number, interatomic spacing) → formation of dimer and trimer type cation-oxygen vacancies defect complex (intrinsic and extrinsic) → dissociation of oxygen vacancies from defect cluster → ionic conductivity temperature. It ismore » a strategic approach to understand key physics of ionic conductivity mechanism in order to reduce operating temperature of electrolytes for intermediate temperature (300–450 °C) electrochemical devices for the first time.« less

MMX-I: A data-processing software for multi-modal X-ray imaging and tomography

NASA Astrophysics Data System (ADS)

Bergamaschi, A.; Medjoubi, K.; Messaoudi, C.; Marco, S.; Somogyi, A.

2017-06-01

Scanning hard X-ray imaging allows simultaneous acquisition of multimodal information, including X-ray fluorescence, absorption, phase and dark-field contrasts, providing structural and chemical details of the samples. Combining these scanning techniques with the infrastructure developed for fast data acquisition at Synchrotron Soleil permits to perform multimodal imaging and tomography during routine user experiments at the Nanoscopium beamline. A main challenge of such imaging techniques is the online processing and analysis of the generated very large volume (several hundreds of Giga Bytes) multimodal data-sets. This is especially important for the wide user community foreseen at the user oriented Nanoscopium beamline (e.g. from the fields of Biology, Life Sciences, Geology, Geobiology), having no experience in such data-handling. MMX-I is a new multi-platform open-source freeware for the processing and reconstruction of scanning multi-technique X-ray imaging and tomographic datasets. The MMX-I project aims to offer, both expert users and beginners, the possibility of processing and analysing raw data, either on-site or off-site. Therefore we have developed a multi-platform (Mac, Windows and Linux 64bit) data processing tool, which is easy to install, comprehensive, intuitive, extendable and user-friendly. MMX-I is now routinely used by the Nanoscopium user community and has demonstrated its performance in treating big data.

New Homogeneous Standards by Atomic Layer Deposition for Synchrotron X-ray Fluorescence and Absorption Spectroscopies.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Butterworth, A.L.; Becker, N.; Gainsforth, Z.

2012-03-13

Quantification of synchrotron XRF analyses is typically done through comparisons with measurements on the NIST SRM 1832/1833 thin film standards. Unfortunately, these standards are inhomogeneous on small scales at the tens of percent level. We are synthesizing new homogeneous multilayer standards using the Atomic Layer Deposition technique and characterizing them using multiple analytical methods, including ellipsometry, Rutherford Back Scattering at Evans Analytical, Synchrotron X-ray Fluorescence (SXRF) at Advanced Photon Source (APS) Beamline 13-ID, Synchrotron X-ray Absorption Spectroscopy (XAS) at Advanced Light Source (ALS) Beamlines 11.0.2 and 5.3.2.1 and by electron microscopy techniques. Our motivation for developing much-needed cross-calibration of synchrotronmore » techniques is borne from coordinated analyses of particles captured in the aerogel of the NASA Stardust Interstellar Dust Collector (SIDC). The Stardust Interstellar Dust Preliminary Examination (ISPE) team have characterized three sub-nanogram, {approx}1{micro}m-sized fragments considered as candidates to be the first contemporary interstellar dust ever collected, based on their chemistries and trajectories. The candidates were analyzed in small wedges of aerogel in which they were extracted from the larger collector, using high sensitivity, high spatial resolution >3 keV synchrotron x-ray fluorescence spectroscopy (SXRF) and <2 keV synchrotron x-ray transmission microscopy (STXM) during Stardust ISPE. The ISPE synchrotron techniques have complementary capabilities. Hard X-ray SXRF is sensitive to sub-fg mass of elements Z {ge} 20 (calcium) and has a spatial resolution as low as 90nm. X-ray Diffraction data were collected simultaneously with SXRF data. Soft X-ray STXM at ALS beamline 11.0.2 can detect fg-mass of most elements, including cosmochemically important oxygen, magnesium, aluminum and silicon, which are invisible to SXRF in this application. ALS beamline 11.0.2 has spatial resolution better than 25 nm. Limiting factors for Stardust STXM analyses were self-imposed limits of photon dose due to radiation damage concerns, and significant attenuation of <1500 eV X-rays by {approx}80{micro}m thick, {approx}25 mg/cm{sup 3} density silica aerogel capture medium. In practice, the ISPE team characterized the major, light elements using STXM (O, Mg, Al, Si) and the heavier minor and trace elements using SXRF. The two data sets overlapped only with minor Fe and Ni ({approx}1% mass abundance), providing few quantitative cross-checks. New improved standards for cross calibration are essential for consortium-based analyses of Stardust interstellar and cometary particles, IDPs. Indeed, they have far reaching application across the whole synchrotron-based analytical community. We have synthesized three ALD multilayers simultaneously on silicon nitride membranes and silicon and characterized them using RBS (on Si), XRF (on Si{sub 3}N{sub 4}) and STXM/XAS (holey Si{sub 3}N{sub 4}). The systems we have started to work with are Al-Zn-Fe and Y-Mg-Er. We have found these ALD multi-layers to be uniform at {micro}m- to nm scales, and have found excellent consistency between four analytical techniques so far. The ALD films can also be used as a standard for e-beam instruments, eg., TEM EELS or EDX. After some early issues with the consistency of coatings to the back-side of the membrane windows, we are confident to be able to show multi-analytical agreement to within 10%. As the precision improves, we can use the new standards to verify or improve the tabulated cross-sections.« less

Diamond sensors and polycapillary lenses for X-ray absorption spectroscopy.

PubMed

Ravel, B; Attenkofer, K; Bohon, J; Muller, E; Smedley, J

2013-10-01

Diamond sensors are evaluated as incident beam monitors for X-ray absorption spectroscopy experiments. These single crystal devices pose a challenge for an energy-scanning experiment using hard X-rays due to the effect of diffraction from the crystalline sensor at energies which meet the Bragg condition. This problem is eliminated by combination with polycapillary lenses. The convergence angle of the beam exiting the lens is large compared to rocking curve widths of the diamond. A ray exiting one capillary from the lens meets the Bragg condition for any reflection at a different energy from the rays exiting adjacent capillaries. This serves to broaden each diffraction peak over a wide energy range, allowing linear measurement of incident intensity over the range of the energy scan. Extended X-ray absorption fine structure data are measured with a combination of a polycapillary lens and a diamond incident beam monitor. These data are of comparable quality to data measured without a lens and with an ionization chamber monitoring the incident beam intensity.

Hydrogen-bearing iron peroxide and its implications to the deep Earth

NASA Astrophysics Data System (ADS)

Liu, J.; Hu, Q.; Kim, D. Y.; Wu, Z.; Wang, W.; Alp, E. E.; Yang, L.; Xiao, Y.; Meng, Y.; Chow, P.; Greenberg, E.; Prakapenka, V. B.; Mao, H. K.; Mao, W. L.

2017-12-01

Hydrous materials subducted into the deep mantle may play a significant role in the geophysical and geochemical processes of the lower mantle through geological time, but their roles have not become clear yet in the region. Hydrogen-bearing iron peroxide (FeO2Hx) was recently discovered to form through dehydrogenation of goethite (e.g., FeOOH) and the reaction between hematite (Fe2O3) and water under deep lower mantle conditions. We conducted synchrotron Mössbauer, X-ray absorption, and X-ray emission spectroscopy measurements to investigate the electronic spin and valence states of iron in hydrogen-bearing iron peroxide (FeO2Hx) in-situ at high pressures. Combined with theoretical calculations and other high-pressure experiments (i.e., nuclear resonant inelastic x-ray scattering spectroscopy and X-ray diffraction coupled with laser-heated diamond-anvil cell techniques), we find that the intriguing properties of FeO2Hx could shed light on the origin of a number of the observed geochemical and geophysical anomalies in the deep Earth.

X-ray computed tomography of wood-adhesive bondlines: Attenuation and phase-contrast effects

DOE PAGES

Paris, Jesse L.; Kamke, Frederick A.; Xiao, Xianghui

2015-07-29

Microscale X-ray computed tomography (XCT) is discussed as a technique for identifying 3D adhesive distribution in wood-adhesive bondlines. Visualization and material segmentation of the adhesives from the surrounding cellular structures require sufficient gray-scale contrast in the reconstructed XCT data. Commercial wood-adhesive polymers have similar chemical characteristics and density to wood cell wall polymers and therefore do not provide good XCT attenuation contrast in their native form. Here, three different adhesive types, namely phenol formaldehyde, polymeric diphenylmethane diisocyanate, and a hybrid polyvinyl acetate, are tagged with iodine such that they yield sufficient X-ray attenuation contrast. However, phase-contrast effects at material edgesmore » complicate image quality and segmentation in XCT data reconstructed with conventional filtered backprojection absorption contrast algorithms. A quantitative phase retrieval algorithm, which isolates and removes the phase-contrast effect, was demonstrated. The paper discusses and illustrates the balance between material X-ray attenuation and phase-contrast effects in all quantitative XCT analyses of wood-adhesive bondlines.« less

Optical control of hard X-ray polarization by electron injection in a laser wakefield accelerator

PubMed Central

Schnell, Michael; Sävert, Alexander; Uschmann, Ingo; Reuter, Maria; Nicolai, Maria; Kämpfer, Tino; Landgraf, Björn; Jäckel, Oliver; Jansen, Oliver; Pukhov, Alexander; Kaluza, Malte Christoph; Spielmann, Christian

2013-01-01

Laser-plasma particle accelerators could provide more compact sources of high-energy radiation than conventional accelerators. Moreover, because they deliver radiation in femtosecond pulses, they could improve the time resolution of X-ray absorption techniques. Here we show that we can measure and control the polarization of ultra-short, broad-band keV photon pulses emitted from a laser-plasma-based betatron source. The electron trajectories and hence the polarization of the emitted X-rays are experimentally controlled by the pulse-front tilt of the driving laser pulses. Particle-in-cell simulations show that an asymmetric plasma wave can be driven by a tilted pulse front and a non-symmetric intensity distribution of the focal spot. Both lead to a notable off-axis electron injection followed by collective electron–betatron oscillations. We expect that our method for an all-optical steering is not only useful for plasma-based X-ray sources but also has significance for future laser-based particle accelerators. PMID:24026068

X-ray computed tomography of wood-adhesive bondlines: Attenuation and phase-contrast effects

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paris, Jesse L.; Kamke, Frederick A.; Xiao, Xianghui

Microscale X-ray computed tomography (XCT) is discussed as a technique for identifying 3D adhesive distribution in wood-adhesive bondlines. Visualization and material segmentation of the adhesives from the surrounding cellular structures require sufficient gray-scale contrast in the reconstructed XCT data. Commercial wood-adhesive polymers have similar chemical characteristics and density to wood cell wall polymers and therefore do not provide good XCT attenuation contrast in their native form. Here, three different adhesive types, namely phenol formaldehyde, polymeric diphenylmethane diisocyanate, and a hybrid polyvinyl acetate, are tagged with iodine such that they yield sufficient X-ray attenuation contrast. However, phase-contrast effects at material edgesmore » complicate image quality and segmentation in XCT data reconstructed with conventional filtered backprojection absorption contrast algorithms. A quantitative phase retrieval algorithm, which isolates and removes the phase-contrast effect, was demonstrated. The paper discusses and illustrates the balance between material X-ray attenuation and phase-contrast effects in all quantitative XCT analyses of wood-adhesive bondlines.« less

Preliminary studies of enhanced contrast radiography in anatomy and embryology of insects with Elettra synchrotron light

NASA Astrophysics Data System (ADS)

Hönnicke, M. G.; Foerster, L. A.; Navarro-Silva, M. A.; Menk, R.-H.; Rigon, L.; Cusatis, C.

2005-08-01

Enhanced contrast X-ray imaging is achieved by exploiting the real part of the refraction index, which is responsible for the phase shifts, in addition to the imaginary part, which is responsible for the absorption. Such techniques are called X-ray phase contrast imaging. An analyzer-based X-ray phase contrast imaging set-up with Diffraction Enhanced Imaging processing (DEI) were used for preliminary studies in anatomy and embryology of insects. Parasitized stinkbug and moth eggs used as control agents of pests in vegetables and adult stinkbugs and mosquitoes ( Aedes aegypti) were used as samples. The experimental setup was mounted in the SYRMEP beamline at ELETTRA. Images were obtained using a high spatial resolution CCD detector (pixel size 14×14 μm 2) coupled with magnifying optics. Analyzer-based X-ray phase contrast images (PCI) and edge detection images show contrast and details not observed with conventional synchrotron radiography and open the possibility for future study in the embryonic development of insects.

Soft X-ray absorption spectroscopy and resonant inelastic X-ray scattering spectroscopy below 100 eV: probing first-row transition-metal M-edges in chemical complexes

PubMed Central

Wang, Hongxin; Young, Anthony T.; Guo, Jinghua; Cramer, Stephen P.; Friedrich, Stephan; Braun, Artur; Gu, Weiwei

2013-01-01

X-ray absorption and scattering spectroscopies involving the 3d transition-metal K- and L-edges have a long history in studying inorganic and bioinorganic molecules. However, there have been very few studies using the M-edges, which are below 100 eV. Synchrotron-based X-ray sources can have higher energy resolution at M-edges. M-edge X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) could therefore provide complementary information to K- and L-edge spectroscopies. In this study, M 2,3-edge XAS on several Co, Ni and Cu complexes are measured and their spectral information, such as chemical shifts and covalency effects, are analyzed and discussed. In addition, M 2,3-edge RIXS on NiO, NiF2 and two other covalent complexes have been performed and different d–d transition patterns have been observed. Although still preliminary, this work on 3d metal complexes demonstrates the potential to use M-edge XAS and RIXS on more complicated 3d metal complexes in the future. The potential for using high-sensitivity and high-resolution superconducting tunnel junction X-ray detectors below 100 eV is also illustrated and discussed. PMID:23765304

Soft X-ray absorption spectroscopy and resonant inelastic X-ray scattering spectroscopy below 100 eV: probing first-row transition-metal M-edges in chemical complexes.

PubMed

Wang, Hongxin; Young, Anthony T; Guo, Jinghua; Cramer, Stephen P; Friedrich, Stephan; Braun, Artur; Gu, Weiwei

2013-07-01

X-ray absorption and scattering spectroscopies involving the 3d transition-metal K- and L-edges have a long history in studying inorganic and bioinorganic molecules. However, there have been very few studies using the M-edges, which are below 100 eV. Synchrotron-based X-ray sources can have higher energy resolution at M-edges. M-edge X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) could therefore provide complementary information to K- and L-edge spectroscopies. In this study, M2,3-edge XAS on several Co, Ni and Cu complexes are measured and their spectral information, such as chemical shifts and covalency effects, are analyzed and discussed. In addition, M2,3-edge RIXS on NiO, NiF2 and two other covalent complexes have been performed and different d-d transition patterns have been observed. Although still preliminary, this work on 3d metal complexes demonstrates the potential to use M-edge XAS and RIXS on more complicated 3d metal complexes in the future. The potential for using high-sensitivity and high-resolution superconducting tunnel junction X-ray detectors below 100 eV is also illustrated and discussed.

New Developments and Geoscience Applications of Synchrotron Computed Microtomography (Invited)

NASA Astrophysics Data System (ADS)

Rivers, M. L.; Wang, Y.; Newville, M.; Sutton, S. R.; Yu, T.; Lanzirotti, A.

2013-12-01

Computed microtomography is the extension to micron spatial resolution of the CAT scanning technique developed for medical imaging. Synchrotron sources are ideal for the method, since they provide a monochromatic, parallel beam with high intensity. High energy storage rings such as the Advanced Photon Source at Argonne National Laboratory produce x-rays with high energy, high brilliance, and high coherence. All of these factors combine to produce an extremely powerful imaging tool for earth science research. Techniques that have been developed include: - Absorption and phase contrast computed tomography with spatial resolution below one micron. - Differential contrast computed tomography, imaging above and below the absorption edge of a particular element. - High-pressure tomography, imaging inside a pressure cell at pressures above 10GPa. - High speed radiography and tomography, with 100 microsecond temporal resolution. - Fluorescence tomography, imaging the 3-D distribution of elements present at ppm concentrations. - Radiographic strain measurements during deformation at high confining pressure, combined with precise x-ray diffraction measurements to determine stress. These techniques have been applied to important problems in earth and environmental sciences, including: - The 3-D distribution of aqueous and organic liquids in porous media, with applications in contaminated groundwater and petroleum recovery. - The kinetics of bubble formation in magma chambers, which control explosive volcanism. - Studies of the evolution of the early solar system from 3-D textures in meteorites - Accurate crystal size distributions in volcanic systems, important for understanding the evolution of magma chambers. - The equation-of-state of amorphous materials at high pressure using both direct measurements of volume as a function of pressure and also by measuring the change x-ray absorption coefficient as a function of pressure. - The location and chemical speciation of toxic elements such as arsenic and nickel in soils and in plant tissues in contaminated Superfund sites. - The strength of earth materials under the pressure and temperature conditions of the Earth's mantle, providing insights into plate tectonics and the generation of earthquakes.

Interferogram conditioning for improved Fourier analysis and application to X-ray phase imaging by grating interferometry.

PubMed

Montaux-Lambert, Antoine; Mercère, Pascal; Primot, Jérôme

2015-11-02

An interferogram conditioning procedure, for subsequent phase retrieval by Fourier demodulation, is presented here as a fast iterative approach aiming at fulfilling the classical boundary conditions imposed by Fourier transform techniques. Interference fringe patterns with typical edge discontinuities were simulated in order to reveal the edge artifacts that classically appear in traditional Fourier analysis, and were consecutively used to demonstrate the correction efficiency of the proposed conditioning technique. Optimization of the algorithm parameters is also presented and discussed. Finally, the procedure was applied to grating-based interferometric measurements performed in the hard X-ray regime. The proposed algorithm enables nearly edge-artifact-free retrieval of the phase derivatives. A similar enhancement of the retrieved absorption and fringe visibility images is also achieved.

Site partitioning of Cr3+ in the trichroic alexandrite BeAl2O4:Cr3+ crystal: contribution from x-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Bordage, Amélie; Rossano, Stéphanie; Horn, Adolf Heinrich; Fuchs, Yves

2012-06-01

X-ray absorption spectroscopy measurements at the Cr K-edge of a trichroic crystal of alexandrite BeAl2O4:Cr3+ for different orientations of the crystal with respect to the polarization and direction of the x-ray incident beam have been performed. Analysis of the experimental spectra with the help of first-principles calculations of x-ray absorption spectra allowed us to estimate the proportion of chromium Cr3+ cations among the two different octahedral sites of the alexandrite structure (70% in the Cs site-30% in the Ci site). The methodology presented in this work opens up new possibilities in the field of mineralogy for the study of complex minerals containing several sites potentially occupied by several transition elements or for solid solutions.

Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Feng; Liu, Yijin; Yu, Xiqian

Rechargeable battery technologies have ignited major breakthroughs in contemporary society, including but not limited to revolutions in transportation, electronics, and grid energy storage. The remarkable development of rechargeable batteries is largely attributed to in-depth efforts to improve battery electrode and electrolyte materials. There are, however, still intimidating challenges of lower cost, longer cycle and calendar life, higher energy density, and better safety for large scale energy storage and vehicular applications. Further progress with rechargeable batteries may require new chemistries (lithium ion batteries and beyond) and better understanding of materials electrochemistry in the various battery technologies. In the past decade, advancementmore » of battery materials has been complemented by new analytical techniques that are capable of probing battery chemistries at various length and time scales. Synchrotron X-ray techniques stand out as one of the most effective methods that allows for nearly nondestructive probing of materials characteristics such as electronic and geometric structures with various depth sensitivities through spectroscopy, scattering, and imaging capabilities. This article begins with the discussion of various rechargeable batteries and associated important scientific questions in the field, followed by a review of synchrotron X-ray based analytical tools (scattering, spectroscopy and imaging) and their successful applications (ex situ, in situ, and in operando) in gaining fundamental insights into these scientific questions. Furthermore, electron microscopy and spectroscopy complement the detection length scales of synchrotron X-ray tools, and are also discussed towards the end. We highlight the importance of studying battery materials by combining analytical techniques with complementary length sensitivities, such as the combination of X-ray absorption spectroscopy and electron spectroscopy with spatial resolution, because a sole technique may lead to biased and inaccurate conclusions. We then discuss the current progress of experimental design for synchrotron experiments and methods to mitigate beam effects. Finally, a perspective is provided to elaborate how synchrotron techniques can impact the development of next-generation battery chemistries.« less

Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries

DOE PAGES

Lin, Feng; Liu, Yijin; Yu, Xiqian; ...

2017-08-30

Rechargeable battery technologies have ignited major breakthroughs in contemporary society, including but not limited to revolutions in transportation, electronics, and grid energy storage. The remarkable development of rechargeable batteries is largely attributed to in-depth efforts to improve battery electrode and electrolyte materials. There are, however, still intimidating challenges of lower cost, longer cycle and calendar life, higher energy density, and better safety for large scale energy storage and vehicular applications. Further progress with rechargeable batteries may require new chemistries (lithium ion batteries and beyond) and better understanding of materials electrochemistry in the various battery technologies. In the past decade, advancementmore » of battery materials has been complemented by new analytical techniques that are capable of probing battery chemistries at various length and time scales. Synchrotron X-ray techniques stand out as one of the most effective methods that allows for nearly nondestructive probing of materials characteristics such as electronic and geometric structures with various depth sensitivities through spectroscopy, scattering, and imaging capabilities. This article begins with the discussion of various rechargeable batteries and associated important scientific questions in the field, followed by a review of synchrotron X-ray based analytical tools (scattering, spectroscopy and imaging) and their successful applications (ex situ, in situ, and in operando) in gaining fundamental insights into these scientific questions. Furthermore, electron microscopy and spectroscopy complement the detection length scales of synchrotron X-ray tools, and are also discussed towards the end. We highlight the importance of studying battery materials by combining analytical techniques with complementary length sensitivities, such as the combination of X-ray absorption spectroscopy and electron spectroscopy with spatial resolution, because a sole technique may lead to biased and inaccurate conclusions. We then discuss the current progress of experimental design for synchrotron experiments and methods to mitigate beam effects. Finally, a perspective is provided to elaborate how synchrotron techniques can impact the development of next-generation battery chemistries.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ovchinnikova, E. N.; Rogalev, A.; Wilhelm, F.

The local electronic structure of copper ions in a copper metaborate CuB{sub 2}O{sub 4} crystal is studied on the ESRF synchrotron using X-ray absorption polarization-dependent spectroscopy. The X-ray natural circular dichroism near the K absorption edge of copper is measured in the direction that is perpendicular to crystal axis c. The data obtained indicate the presence of hybridized p–d electronic states of copper. Theoretical calculations are used to separate the contributions of the two crystallographically nonequivalent positions of copper atoms in the unit cell of CuB{sub 2}O{sub 4} to the absorption and X-ray circular dichroism spectra of the crystal.

LPE growth and characterization of InAs1-xNx films

NASA Astrophysics Data System (ADS)

Lv, Y. F.; Hu, S. H.; Yang, X. Y.; Wang, Y.; Sun, C. H.; Qiu, F.; Cong, R.; Dong, W. J.; Zhang, Y.; Yu, G. L.; Dai, N.

2014-07-01

A series of InAs1-xNx films have been successfully grown on (100) oriented InAs substrates by liquid phase epitaxy technique. Samples with different nitrogen contents have been analyzed by high-resolution x-ray diffraction measurement, which confirms the incorporation of N in the epilayers. N-related modes are detected in the Raman spectra of InAs1-xNx epilayers. The fundamental absorption edges of InAs1-xNx films obtained by Fourier transform infrared transmission spectroscopy exhibit a red-shift compared with that of InAs homoepilayer.

NARROW LINE ABSORPTION IN CACO3.

DTIC Science & Technology

CARBONATES), (*CALCIUM COMPOUNDS, (*ABSORPTION SPECTRA, CALCITE), (*CALCITE, RADIATION EFFECTS), ELECTRON PARAMAGNETIC RESONANCE, SINGLE CRYSTALS , NEUTRONS, X RAYS, GAMMA RAYS, IONS, CRYSTAL DEFECTS, PARAMAGNETIC RESONANCE.

High-Resolution X-Ray Spectroscopy and Modeling of the Absorbing and Emitting Outflow in NGC 3783

NASA Astrophysics Data System (ADS)

Kaspi, Shai; Brandt, W. N.; Netzer, Hagai; George, Ian M.; Chartas, George; Behar, Ehud; Sambruna, Rita M.; Garmire, Gordon P.; Nousek, John A.

2001-06-01

The high-resolution X-ray spectrum of NGC 3783 shows several dozen absorption lines and a few emission lines from the H-like and He-like ions of O, Ne, Mg, Si, and S, as well as from Fe XVII-Fe XXIII L-shell transitions. We have reanalyzed the Chandra HETGS spectrum using better flux and wavelength calibrations, along with more robust methods. Combining several lines from each element, we clearly demonstrate the existence of the absorption lines and determine that they are blueshifted relative to the systemic velocity by -610+/-130 km s-1. We find the Ne absorption lines in the High-Energy Grating spectrum to be resolved with FWHM=840+490-360 km s-1; no other lines are resolved. The emission lines are consistent with being at the systemic velocity. We have used regions in the spectrum where no lines are expected to determine the X-ray continuum, and we model the absorption and emission lines using photoionized-plasma calculations. The model consists of two absorption components, with different covering factors, which have an order-of-magnitude difference in their ionization parameters. The two components are spherically outflowing from the active galactic nucleus, and thus contribute to both the absorption and the emission via P Cygni profiles. The model also clearly requires O VII and O VIII absorption edges. The low-ionization component of our model can plausibly produce UV absorption lines with equivalent widths consistent with those observed from NGC 3783. However, we note that this result is highly sensitive to the unobservable UV to X-ray continuum, and the available UV and X-ray observations cannot firmly establish the relationship between the UV and X-ray absorbers. We find good agreement between the Chandra spectrum and simultaneous ASCA and RXTE observations. The 1 keV deficit previously found when modeling ASCA data probably arises from iron L-shell absorption lines not included in previous models. We also set an upper limit on the FWHM of the narrow Fe Kα emission line of 3250 km s-1. This is consistent with this line originating outside the broad-line region, possibly from a torus.

Preparation of γ-LiV2O5 from polyoxovanadate cluster Li7[V15O36(CO3)] as a high-performance cathode material and its reaction mechanism revealed by operando XAFS

NASA Astrophysics Data System (ADS)

Wang, Heng; Isobe, Jin; Shimizu, Takeshi; Matsumura, Daiju; Ina, Toshiaki; Yoshikawa, Hirofumi

2017-08-01

γ-phase LiV2O5, which shows superior electrochemical performance as cathode material in Li-ion batteries, was prepared by annealing the polyoxovanadate cluster Li7 [V15O36(CO3)]. The reaction mechanism was studied using operando X-ray absorption fine structure (XAFS), powder X-ray diffraction (PXRD), and X-ray photoelectron spectroscopy (XPS) analyses. The X-ray absorption near edge structure (XANES) and XPS results reveal that γ-LiV2O5 undergoes two-electron redox reaction per V2O5 pyramid unit, resulting in a large reversible capacity of 260 Ah/kg. The extended X-ray absorption fine structure (EXAFS) and PXRD analyses also suggest that the V-V distance slightly increases, due to the reduction of V5+ to V4+ during Li ion intercalation as the material structure is maintained. As a result, γ-LixV2O5 shows highly reversible electrochemical reaction with x = 0.1-1.9.

In-situ X-Ray Absorption Spectroscopy (XAS) Investigation of a Bifunctional Manganese Oxide Catalyst with High Activity for Electrochemical Water Oxidation and Oxygen Reduction

PubMed Central

Benck, Jesse D.; Gul, Sheraz; Webb, Samuel M.; Yachandra, Vittal K.; Yano, Junko; Jaramillo, Thomas F.

2013-01-01

In-situ x-ray absorption spectroscopy (XAS) is a powerful technique that can be applied to electrochemical systems, with the ability to elucidate the chemical nature of electrocatalysts under reaction conditions. In this study, we perform in-situ XAS measurements on a bifunctional manganese oxide (MnOx) catalyst with high electrochemical activity for the oxygen reduction reaction (ORR) and the oxygen evolution reaction (OER). Using x-ray absorption near edge structure (XANES) and extended x-ray absorption fine structure (EXAFS), we find that exposure to an ORR-relevant potential of 0.7 V vs. RHE produces a disordered Mn3II,III,IIIO4 phase with negligible contributions from other phases. After the potential is increased to a highly anodic value of 1.8 V vs. RHE, relevant to the OER, we observe an oxidation of approximately 80% of the catalytic thin film to form a mixed MnIII,IV oxide, while the remaining 20% of the film consists of a less oxidized phase, likely corresponding to unchanged Mn3II,III,IIIO4. XAS and electrochemical characterization of two thin film catalysts with different MnOx thicknesses reveals no significant influence of thickness on the measured oxidation states, at either ORR or OER potentials, but demonstrates that the OER activity scales with film thickness. This result suggests that the films have porous structure, which does not restrict electrocatalysis to the top geometric layer of the film. As the portion of the catalyst film that is most likely to be oxidized at the high potentials necessary for the OER is that which is closest to the electrolyte interface, we hypothesize that the MnIII,IV oxide, rather than Mn3II,III,IIIO4, is the phase pertinent to the observed OER activity. PMID:23758050

Discovery of a dual active galactic nucleus with ˜8 kpc separation

NASA Astrophysics Data System (ADS)

Ellison, Sara L.; Secrest, Nathan J.; Mendel, J. Trevor; Satyapal, Shobita; Simard, Luc

2017-09-01

Targeted searches for dual active galactic nuclei (AGNs), with separations 1-10 kpc, have yielded relatively few successes. A recent pilot survey by Satyapal et al. has demonstrated that mid-infrared (mid-IR) pre-selection has the potential to significantly improve the success rate for dual AGN confirmation in late stage galaxy mergers. In this Letter, we combine mid-IR selection with spatially resolved optical AGN diagnostics from the Mapping Nearby Galaxies at Apache Point Observatory survey to identify a candidate dual AGN in the late stage major galaxy merger SDSS J140737.17+442856.2 at z = 0.143. The nature of the dual AGN is confirmed with Chandra X-ray observations that identify two hard X-ray point sources with intrinsic (corrected for absorption) 2-10 keV luminosities of 4 × 1041 and 3.5 × 1043 erg s-1 separated by 8.3 kpc. The neutral hydrogen absorption (˜1022 cm-2) towards the two AGNs is lower than in duals selected solely on their mid-IR colours, indicating that strategies that combine optical and mid-IR diagnostics may complement techniques that identify the highly obscured dual phase, such as at high X-ray energies or mid-IR only.

Tables of X-ray absorption corrections and dispersion corrections: the new versus the old

NASA Astrophysics Data System (ADS)

Creagh, Dudley

1990-11-01

This paper compares the data on X-ray absorption coefficients calculated by Creagh and Hubbell and tabulated in International Tables for Crystallography, vol. C, ed. A.J.C. Wilson (1990) section 4.2.4 [1] with empirical (Saloman, Hubbell and Scofield, At. Data and Nucl. Data Tables 38 (1988) 1, [6]) and semi-empirical (Hubbell, McMaster, Kerr Del Grande and Mallett, in: International Tables for Crystallography, vol. IV, eds. Ibers and Hamilton (Kynoch, Birmingham, 1974) [2]) tabulations as well as the renormalized relativistic Dirac-Hartree-Fock calculations of Scofield [6]. It also makes comparisons of the real part of the dispersion correction ƒ‧(ω, 0) and tabulated in ref. [1], with theoretical data sets (Cromer and Liberman, J. Chem. Phys. 53 (1970) 1891, and Acta Crystallogr. A37 (1981) 267 [4,5]; Wang, Phys. Rev. A34 (1986) 636 [85]; Kissel, in: Workshop Report on New Dimensions in X-ray Scattering, CONF-870459 (Livermore, 1987) p. 9 [86]) and data collected using a variety of experimental techniques. In both cases the data tabulated in ref. [1] is shown to give improved self-consistency and agreement with experiment.

X-ray imaging of spin currents and magnetisation dynamics at the nanoscale

NASA Astrophysics Data System (ADS)

Bonetti, Stefano

2017-04-01

Understanding how spins move in time and space is the aim of both fundamental and applied research in modern magnetism. Over the past three decades, research in this field has led to technological advances that have had a major impact on our society, while improving the understanding of the fundamentals of spin physics. However, important questions still remain unanswered, because it is experimentally challenging to directly observe spins and their motion with a combined high spatial and temporal resolution. In this article, we present an overview of the recent advances in x-ray microscopy that allow researchers to directly watch spins move in time and space at the microscopically relevant scales. We discuss scanning x-ray transmission microscopy (STXM) at resonant soft x-ray edges, which is available at most modern synchrotron light sources. This technique measures magnetic contrast through the x-ray magnetic circular dichroism (XMCD) effect at the resonant absorption edges, while focusing the x-ray radiation at the nanometre scale, and using the intrinsic pulsed structure of synchrotron-generated x-rays to create time-resolved images of magnetism at the nanoscale. In particular, we discuss how the presence of spin currents can be detected by imaging spin accumulation, and how the magnetisation dynamics in thin ferromagnetic films can be directly imaged. We discuss how a direct look at the phenomena allows for a deeper understanding of the the physics at play, that is not accessible to other, more indirect techniques. Finally, we present an overview of the exciting opportunities that lie ahead to further understand the fundamentals of novel spin physics, opportunities offered by the appearance of diffraction limited storage rings and free electron lasers.

X-ray imaging of spin currents and magnetisation dynamics at the nanoscale.

PubMed

Bonetti, Stefano

2017-04-05

Understanding how spins move in time and space is the aim of both fundamental and applied research in modern magnetism. Over the past three decades, research in this field has led to technological advances that have had a major impact on our society, while improving the understanding of the fundamentals of spin physics. However, important questions still remain unanswered, because it is experimentally challenging to directly observe spins and their motion with a combined high spatial and temporal resolution. In this article, we present an overview of the recent advances in x-ray microscopy that allow researchers to directly watch spins move in time and space at the microscopically relevant scales. We discuss scanning x-ray transmission microscopy (STXM) at resonant soft x-ray edges, which is available at most modern synchrotron light sources. This technique measures magnetic contrast through the x-ray magnetic circular dichroism (XMCD) effect at the resonant absorption edges, while focusing the x-ray radiation at the nanometre scale, and using the intrinsic pulsed structure of synchrotron-generated x-rays to create time-resolved images of magnetism at the nanoscale. In particular, we discuss how the presence of spin currents can be detected by imaging spin accumulation, and how the magnetisation dynamics in thin ferromagnetic films can be directly imaged. We discuss how a direct look at the phenomena allows for a deeper understanding of the the physics at play, that is not accessible to other, more indirect techniques. Finally, we present an overview of the exciting opportunities that lie ahead to further understand the fundamentals of novel spin physics, opportunities offered by the appearance of diffraction limited storage rings and free electron lasers.

Noninvasive Synchrotron-Based X-ray Raman Scattering Discriminates Carbonaceous Compounds in Ancient and Historical Materials [ In situ synchrotron-based X-Ray Raman scattering discriminates carbonaceous compounds in ancient and historical materials

DOE PAGES

Gueriau, Pierre; Rueff, Jean -Pascal; Bernard, Sylvain; ...

2017-09-13

Carbon compounds are ubiquitous and occur in a diversity of chemical forms in many systems including ancient and historic materials ranging from cultural heritage to paleontology. Determining their speciation cannot only provide unique information on their origin but may also elucidate degradation processes. Synchrotron-based X-ray absorption near-edge structure (XANES) spectroscopy at the carbon K-edge (280–350 eV) is a very powerful method to probe carbon speciation. However, the short penetration depth of soft X-rays imposes stringent constraints on sample type, preparation, and analytical environment. A hard X-ray probe such as X-ray Raman scattering (XRS) can overcome many of these difficulties. Heremore » we report the use of XRS at ~6 keV incident energy to collect carbon K-edge XANES data and probe the speciation of organic carbon in several specimens relevant to cultural heritage and natural history. This methodology enables the measurement to be done in a nondestructive way, in air, and provides information that is not compromised by surface contamination by ensuring that the dominant signal contribution is from the bulk of the probed material. Using the backscattering geometry at large photon momentum transfer maximizes the XRS signal at the given X-ray energy and enhances nondipole contributions compared to conventional XANES, thereby augmenting the speciation sensitivity. The capabilities and limitations of the technique are discussed. As a result, we show that despite its small cross section, for a range of systems the XRS method can provide satisfactory signals at realistic experimental conditions. XRS constitutes a powerful complement to FT-IR, Raman, and conventional XANES spectroscopy, overcoming some of the limitations of these techniques.« less

CAT-ACT—A new highly versatile x-ray spectroscopy beamline for catalysis and radionuclide science at the KIT synchrotron light facility ANKA

NASA Astrophysics Data System (ADS)

Zimina, A.; Dardenne, K.; Denecke, M. A.; Doronkin, D. E.; Huttel, E.; Lichtenberg, H.; Mangold, S.; Pruessmann, T.; Rothe, J.; Spangenberg, Th.; Steininger, R.; Vitova, T.; Geckeis, H.; Grunwaldt, J.-D.

2017-11-01

CAT-ACT—the hard X-ray beamline for CATalysis and ACTinide/radionuclide research at the KIT synchrotron radiation facility ANKA—is dedicated to X-ray spectroscopy, including "flux hungry" photon-in/photon-out and correlative techniques and combines state-of-the-art optics with a unique infrastructure for radionuclide and catalysis research. Measurements can be performed at photon energies varying between 3.4 keV and 55 keV, thus encompassing the actinide M- and L-edge or potassium K-edge up to the K-edges of the lanthanide series such as cerium. Well-established X-ray absorption fine structure spectroscopy in transmission and fluorescence detection modes is available in combination with high energy-resolution X-ray emission spectroscopy or X-ray diffraction techniques. The modular beamline design with two alternately operated in-line experimental stations enables sufficient flexibility to adapt sample environments and detection systems to many scientific challenges. The ACT experimental station focuses on various aspects of nuclear waste disposal within the mission of the Helmholtz association to contribute to the solution of one of the greatest scientific and social challenges of our time—the safe disposal of heat producing, highly radioactive waste forms from nuclear energy production. It augments present capabilities at the INE-Beamline by increasing the flux and extending the energy range into the hard X-ray regime. The CAT experimental station focuses on catalytic materials, e.g., for energy-related and exhaust gas catalysis. Characterization of catalytically active materials under realistic reaction conditions and the development of in situ and operando cells for sample environments close to industrial reactors are essential aspects at CAT.

CAT-ACT-A new highly versatile x-ray spectroscopy beamline for catalysis and radionuclide science at the KIT synchrotron light facility ANKA.

PubMed

Zimina, A; Dardenne, K; Denecke, M A; Doronkin, D E; Huttel, E; Lichtenberg, H; Mangold, S; Pruessmann, T; Rothe, J; Spangenberg, Th; Steininger, R; Vitova, T; Geckeis, H; Grunwaldt, J-D

2017-11-01

CAT-ACT-the hard X-ray beamline for CATalysis and ACTinide/radionuclide research at the KIT synchrotron radiation facility ANKA-is dedicated to X-ray spectroscopy, including "flux hungry" photon-in/photon-out and correlative techniques and combines state-of-the-art optics with a unique infrastructure for radionuclide and catalysis research. Measurements can be performed at photon energies varying between 3.4 keV and 55 keV, thus encompassing the actinide M- and L-edge or potassium K-edge up to the K-edges of the lanthanide series such as cerium. Well-established X-ray absorption fine structure spectroscopy in transmission and fluorescence detection modes is available in combination with high energy-resolution X-ray emission spectroscopy or X-ray diffraction techniques. The modular beamline design with two alternately operated in-line experimental stations enables sufficient flexibility to adapt sample environments and detection systems to many scientific challenges. The ACT experimental station focuses on various aspects of nuclear waste disposal within the mission of the Helmholtz association to contribute to the solution of one of the greatest scientific and social challenges of our time-the safe disposal of heat producing, highly radioactive waste forms from nuclear energy production. It augments present capabilities at the INE-Beamline by increasing the flux and extending the energy range into the hard X-ray regime. The CAT experimental station focuses on catalytic materials, e.g., for energy-related and exhaust gas catalysis. Characterization of catalytically active materials under realistic reaction conditions and the development of in situ and operando cells for sample environments close to industrial reactors are essential aspects at CAT.

Through BAL Quasars Brightly

NASA Technical Reports Server (NTRS)

Chartas, George

2003-01-01

We report on an observation of the broad absorption line (BAL) quasar PG 1115+080 performed with the XMM-Newton observatory. Spectral analysis reveals the second case of a relativistic X-ray-absorbing outflow in a BAL quasar. The first case was revealed in a recent observation of APM 08279+5255 with the Chandra X-Ray Observatory. As in the case of APM 08279+5255, the observed flux of PG 1115+080 is greatly magnified by gravitational lensing. The relatively high redshift (z=1.72) of the quasar places the redshifted energies of resonant absorption features in a sensitive portion of the XMM- Newton spectral response. The spectrum indicates the presence of complex low-energy absorption in the 0.2-0.6 keV observed energy band and high-energy absorption in the 2-5 keV observed energy band. The high-energy absorption is best modeled by two Gaussian absorption lines with rest-frame energies of 7.4 and 9.5 keV. Assuming that these two lines axe produced by resonant absorption due to Fe XXV, we infer that the X-ray absorbers are outflowing with velocities of approx. 0.10c and approx. 0.34c respectively. We have detected significant variability of the energies and widths of the X-ray BALs in PG 1115+080 and APM 08279+5255 over timescales of 19 and 1.8 weeks (proper time), respectively. The BAL variability observed from APM 08279+5255 supports our earlier conclusion that these absorbers are most likely launched at relatively small radii of less than 10(exp 16)(Mbh/M8)(sup 1/2) cm. A comparison of the ionization properties and column densities of the low-energy and high-energy absorbers indicates that these absorbers are likely distinct; however, higher spectral resolution is needed to confirm this result. Finally, we comment on prospects for constraining the kinematic and ionization properties of these X-ray BALs with the next generation of X-ray observatories.

Ionospheric Absorption on 1539 Khz in Relation to Solar Ionizing Radiation

NASA Technical Reports Server (NTRS)

Boska, J.

1984-01-01

Radio wave absorption data on 1539 kHz for the summer period of 1978 to 1980 are considered in relation to variations of solar X-ray and L-alpha radiation. It is shown that under non-flare conditions L-alpha dominates in controlling absorption and that X-rays contribute about 10% to the total absorption. Optimum regression equations show that absorption is proportional to the m-th power of ionizing flux where m 1. The role of correcting L-alpha values, measured by the AE-E satellite, is discussed.

600 eV falcon-linac thomson x-ray source

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crane, J K; LeSage, G P; Ditmire, T

2000-12-15

The advent of 3rd generation light sources such as the Advanced Light Source (ALS) at LBL, and the Advanced Photon Source at Argonne, have produced a revolution in x-ray probing of dense matter during the past decade. These machines use electron-synchrotrons in conjunction with undulator stages to produce 100 psec x-ray pulses with photon energies of several kiloelectronvolts (keV). The applications for x-ray probing of matter are numerous and diverse with experiments in medicine and biology, semiconductors and materials science, and plasma and solid state physics. In spite of the success of the 3rd generation light sources there is strongmore » motivation to push the capabilities of x-ray probing into new realms, requiring shorter pulses, higher brightness and harder x-rays. A 4th generation light source, the Linac Coherent Light Source (LCLS), is being considered at the Stanford Linear Accelerator [1]. The LCLS will produce multi-kilovolt x-rays of subpicosecond duration that are 10 orders of magnitude brighter than today's 3rd generation light sources.[1] Although the LCLS will provide unprecedented capability for performing time-resolved x-ray probing of ultrafast phenomena at solid densities, this machine will not be completed for many years. In the meantime there is a serious need for an ultrashort-pulse, high-brightness, hard x-ray source that is capable of probing deep into high-Z solid materials to measure dynamic effects that occur on picosecond time scales. Such an instrument would be ideal for probing the effects of shock propagation in solids using Bragg and Laue diffraction. These techniques can be used to look at phase transitions, melting and recrystallization, and the propagation of defects and dislocations well below the surface in solid materials. [2] These types of dynamic phenomena undermine the mechanical properties of metals and are of general interest in solid state physics, materials science, metallurgy, and have specific relevance to stockpile stewardship. Another x-ray diagnostic technique, extended x-ray absorption fine structure (EXAFS) spectroscopy, can be used to measure small-scale structural changes to understand the underlying atomic physics associated with the formation of defects. [2]« less

Time-dependent nonequilibrium soft x-ray response during a spin crossover

NASA Astrophysics Data System (ADS)

van Veenendaal, Michel

2018-03-01

A theoretical framework is developed for better understanding the time-dependent soft-x-ray response of dissipative quantum many-body systems. It is shown how x-ray absorption and resonant inelastic x-ray scattering (RIXS) at transition-metal L edges can provide insight into ultrafast intersystem crossings of importance for energy conversion, ultrafast magnetism, and catalysis. The photoinduced doublet-to-quartet spin crossover on cobalt in Fe-Co Prussian blue analogs is used as a model system to demonstrate how the x-ray response is affected by the nonequilibrium dynamics on a femtosecond time scale. Changes in local spin and symmetry and the underlying mechanism are reflected in strong broadenings, a collapse of clear selection rules during the intersystem crossing, fluctuations in the isotropic branching ratio in x-ray absorption, crystal-field collapse and/or oscillations, and time-dependent anti-Stokes processes in RIXS.

Resonant soft X-ray scattering on protein solutions

NASA Astrophysics Data System (ADS)

Ye, Dan; Le, Thinh; Wang, Cheng; Zwart, Peter; Gomez, Esther; Gomez, Enrique

Protein structure is crucial for biological function, such that characterizing protein folding and packing is important for the design of therapeutics and enzymes. We propose resonant soft X-ray scattering (RSOXS) as an approach to study proteins and other biological assemblies in solution. Calculations of the scattering contrast suggest that soft X-ray scattering is more sensitive than hard X-ray scattering, because of contrast generated at the absorption edges of constituent elements such as carbon, nitrogen and oxygen. We have examined the structure of bovine serum albumin (BSA) in solution by RSOXS. We find that by varying incident X-ray energies, we are able to achieve higher scattering contrast near the absorption edge. From our RSOXS scattering result we are able to reconstruct the structure of BSA in 3D. These RSOXS results also agree with hard X-ray experiments, including crystallographic data. Our study demonstrates the potential of RSOXS for studying protein structure in solution.

Wind-jet interaction in high-mass X-ray binaries

NASA Astrophysics Data System (ADS)

Zdziarski, Andrzej

2016-07-01

Jets in high-mass X-ray binaries can strongly interact with the stellar wind from the donor. The interaction leads, in particular, to formation of recollimation shocks. The shocks can then accelerate electrons in the jet and lead to enhanced emission, observable in the radio and gamma-ray bands. DooSoo, Zdziarski & Heinz (2016) have formulated a condition on the maximum jet power (as a function of the jet velocity and wind rate and velocity) at which such shocks form. This criterion can explain the large difference in the radio and gamma-ray loudness between Cyg X-1 and Cyg X-3. The orbital modulation of radio emission observed in Cyg X-1 and Cyg X-3 allows a measurement of the location of the height along the jet where the bulk of emission at a given frequency occurs. Strong absorption of X-rays in the wind of Cyg X-3 is required to account for properties of the correlation of the radio emission with soft and hard X-rays. That absorption can also account for the unusual spectral and timing X-ray properties of this source.

Synthesis and properties of nanocrystalline copper indium oxide thin films deposited by Rf magnetron sputtering.

PubMed

Singh, Mandeep; Singh, V N; Mehta, B R

2008-08-01

Nanocrystalline copper indium oxide (CuInO2) thin films with particle size ranging from 25 nm to 71 nm have been synthesized from a composite target using reactive Rf magnetron sputtering technique. X-ray photoelectron spectroscopy (XPS) combined with glancing angle X-ray diffraction (GAXRD) analysis confirmed the presence of delafossite CuInO2 phase in these films. The optical absorption studies show the presence of two direct band gaps at 3.3 and 4.3 eV, respectively. The resistance versus temperature measurements show thermally activated hopping with activation energy of 0.84 eV to be the conduction mechanism.

X-ray Experiments for Students at the SLS Optics Beamline

NASA Astrophysics Data System (ADS)

Flechsig, U.; Als-Nielsen, J.; Jaggi, A.; Krempaský, J.; Oberta, P.; Spielmann, S.; van der Veen, J. F.

2010-06-01

We present a X-ray training course for students. The course covers fundamental properties of synchrotron radiation and basic techniques like scattering and absorption. We prepared ten experiments together with a tutorial. The whole course takes about a week. A first student group from the University of Copenhagen passed the course in June 2009. The experiments were performed at the optics beamline of the Swiss Light Source which can be part-time allocated for training purposes. Two experiments are described in more detail: scattering from a hanging drop of water turning into ice and measurement of the power of a pink synchrotron beam using a simple calorimeter.

Effects of X-ray irradiation on the Eu3+ → Eu2+ conversion in CaAl2O4 phosphors

NASA Astrophysics Data System (ADS)

Gomes, Manassés A.; Carvalho, Jéssica C.; Andrade, Adriano B.; Rezende, Marcos V.; Macedo, Zélia S.; Valerio, Mário E. G.

2018-01-01

This paper reports structural and luminescence properties of Eu-doped CaAl2O4 produced by an alternative sol-gel method using coconut water. Results of differential thermal analysis (DTA), thermogravimetric analysis (TGA), and X-ray diffraction (XRD) allowed us to identify the best synthesis conditions for sample preparation. Simultaneous measurements of X-ray absorption spectroscopy (XAS) and X-ray excited optical luminescence (XEOL) were also performed in the X-ray energy range of the Eu LIII edge. Results from photoluminescence (PL) showed only the characteristic Eu3+ emission. However, radioluminescence emission spectra from Eu-doped CaAl2O4 shows a process of conversion of Eu3+ to Eu2+, which is induced by X-ray irradiation and is dependent on the radiation dose energy. X-ray absorption near edge structure (XANES) measurements corroborate Eu reduction due to irradiation, showing that only the Eu3+ ion is present in stable form in the CaAl2O4.

Synchrotron X-ray imaging of nanomagnetism in meteoritic metal (Invited)

NASA Astrophysics Data System (ADS)

Bryson, J. F.; Herrero Albillos, J.; Kronast, F.; Tyliszczak, T.; Redfern, S. A.; van der Laan, G.; Harrison, R. J.

2013-12-01

It is becoming increasingly apparent that a wealth of paleomagnetic information is stored at the nanoscale within natural samples. To date, this nanopaleomagetism has been investigated using high resolution magnetic microscopies, such as electron holography. Although unparalleled in its spatial resolution, electron holography produces images that are indirectly related to the magnetisation state of the sample, introducing ambiguity when interpreting magnetisation information. Holography also requires extensive off-line processing, making it unsuitable for studying dynamic processes, and the sample preparation negates the study of natural remanences. Here we demonstrate the capabilities of a new generation of nanomagnetic imaging methods using synchrotron X-ray radiation. X-rays tuned to an elemental absorption edge can display differing excitation probabilities depending on the orientation of an electron's magnetic moment relative to that of the X-ray beam. This is achieved by introducing an angular momentum to the photon through circular polarisation, resulting in an absorption signal that is proportional to the projection of the magnetic moment on to the X-ray beam direction. We introduce and compare two experimental set-ups capable of spatially resolving these signals to form a high-resolution magnetisation map: photoemission electron microscopy and scanning transmission electron microscopy. Both techniques provide measurements of magnetisation with 30-50nm resolution and elemental specificity. Photoemission electron microscopy can be used also to create maps of all three of the spatial components of magnetisation and investigate dynamic magnetic switching processes. The full capabilities of X-ray imaging are demonstrated through the application of both of these techniques to meteoritic metal. We show that the 'cloudy zone' within iron meteorites contains nanoscale islands of tetrataenite (FeNi) that are populated equally by all three possible magnetic easy axes, suggesting that there were no stray fields (either magnetic or stress) effecting the magnetisation during cloudy zone formation. This observation allows for dynamo field information to be extracted from X-ray nanomagnetic images of the cloudy zone in metallic inclusions within certain chondritic meteorites, as it implies that any deviation from the randomly populated easy axis distribution can be assigned to an external dynamo field. As the cloudy zone forms over 10-100 Ma, this observation suggests that X-ray imaging of the nanopaleomagentism in these meteorites could provide an elegant and concise relative measure of asteroid dynamo field direction and strength over this entire time period, revolutionising our understanding of dynamo processes and planetary formation.

Oxidation and crystal field effects in uranium

NASA Astrophysics Data System (ADS)

Tobin, J. G.; Yu, S.-W.; Booth, C. H.; Tyliszczak, T.; Shuh, D. K.; van der Laan, G.; Sokaras, D.; Nordlund, D.; Weng, T.-C.; Bagus, P. S.

2015-07-01

An extensive investigation of oxidation in uranium has been pursued. This includes the utilization of soft x-ray absorption spectroscopy, hard x-ray absorption near-edge structure, resonant (hard) x-ray emission spectroscopy, cluster calculations, and a branching ratio analysis founded on atomic theory. The samples utilized were uranium dioxide (U O2) , uranium trioxide (U O3) , and uranium tetrafluoride (U F4) . A discussion of the role of nonspherical perturbations, i.e., crystal or ligand field effects, will be presented.

The 16th International Conference on X-ray Absorption Fine Structure (XAFS16)

NASA Astrophysics Data System (ADS)

Grunwaldt, J.-D.; Hagelstein, M.; Rothe, J.

2016-05-01

This preface of the proceedings volume of the 16th International Conference on X- ray Absorption Fine Structure (XAFS16) gives a glance on the five days of cutting-edge X-ray science which were held in Karlsruhe, Germany, August 23 - 28, 2015. In addition, several satellite meetings took place in Hamburg, Berlin and Stuttgart, a Sino-German workshop, three data analysis tutorials as well as special symposia on industrial catalysis and XFELs were held at the conference venue.

Modeling L2,3-Edge X-ray Absorption Spectroscopy with Real-Time Exact Two-Component Relativistic Time-Dependent Density Functional Theory.

PubMed

Kasper, Joseph M; Lestrange, Patrick J; Stetina, Torin F; Li, Xiaosong

2018-04-10

X-ray absorption spectroscopy is a powerful technique to probe local electronic and nuclear structure. There has been extensive theoretical work modeling K-edge spectra from first principles. However, modeling L-edge spectra directly with density functional theory poses a unique challenge requiring further study. Spin-orbit coupling must be included in the model, and a noncollinear density functional theory is required. Using the real-time exact two-component method, we are able to variationally include one-electron spin-orbit coupling terms when calculating the absorption spectrum. The abilities of different basis sets and density functionals to model spectra for both closed- and open-shell systems are investigated using SiCl 4 and three transition metal complexes, TiCl 4 , CrO 2 Cl 2 , and [FeCl 6 ] 3- . Although we are working in the real-time framework, individual molecular orbital transitions can still be recovered by projecting the density onto the ground state molecular orbital space and separating contributions to the time evolving dipole moment.

Radiation effects on beta /10.6/ of pure and europium doped KCl

NASA Technical Reports Server (NTRS)

Grimes, H. H.; Maisel, J. E.; Hartford, R. H.

1975-01-01

Changes in the optical absorption coefficient as the result of X-ray and electron bombardment of pure monocrystalline and polycrystalline KCl and of divalent europium doped polycrystalline KCl were determined. A constant heat flow calorimetric method was used to measure the optical absorption coefficients. Both 300 kV X-ray irradiation and 2 MeV electron irradiation produced increases in the optical absorption coefficient at room temperature. X-ray irradiation produced more significant changes in pure monocrystalline KCl than equivalent amounts of electron irradiation. Electron irradiation of pure and Eu-doped polycrystalline KCl produced increases in the absorption by as much as a factor of 20 over untreated material. Bleaching of the electron-irradiated doped KCl with 649 millimicron light produced a further increase.

Optical nonlinear absorption characteristics of Sb2Se3 nanoparticles

NASA Astrophysics Data System (ADS)

Muralikrishna, Molli; Kiran, Aditha Sai; Ravikanth, B.; Sowmendran, P.; Muthukumar, V. Sai; Venkataramaniah, Kamisetti

2014-04-01

In this work, we report for the first time, the nonlinear optical absorption properties of antimony selenide (Sb2Se3) nanoparticles synthesized through solvothermal route. X-ray diffraction results revealed the crystalline nature of the nanoparticles. Electron microscopy studies revealed that the nanoparticles are in the range of 10 - 40 nm. Elemental analysis was performed using EDAX. By employing open aperture z-scan technique, we have evaluated the effective two-photon absorption coefficient of Sb2Se3 nanoparticles to be 5e-10 m/W at 532 nm. These nanoparticles exhibit strong intensity dependent nonlinear optical absorption and hence could be considered to have optical power limiting applications in the visible range.

Experiment to Determine the Absorption Coefficient of Gamma Rays as a Function of Energy.

ERIC Educational Resources Information Center

Ouseph, P. J.; And Others

1982-01-01

Simpler than x-ray diffractometer experiments, the experiment described illustrates certain concepts regarding the interaction of electromagnetic rays with matter such as the exponential decrease in the intensity with absorber thickness, variation of the coefficient of absorption with energy, and the effect of the K-absorption edge on the…

A study on micro-structural and optical parameters of InxSe1-x thin film

NASA Astrophysics Data System (ADS)

Patel, P. B.; Desai, H. N.; Dhimmar, J. M.; Modi, B. P.

2018-04-01

Thin film of Indium Selenide (InSe) has been deposited by thermal evaporation technique onto pre cleaned glass substrate under high vacuum condition. The micro-structural and optical properties of InxSe1-x (x = 0.6, 1-x = 0.4) thin film have been characterized by X-ray diffractrometer (XRD) and UV-Visible spectrophotometer. The XRD spectra showed that InSe thin film has single phase hexagonal structure with preferred orientation along (1 1 0) direction. The micro-structural parameters (crystallite size, lattice strain, dislocation density, domain population) for InSe thin film have been calculated using XRD spectra. The optical parameters (absorption, transmittance, reflectance, energy band gap, Urbach energy) of InSe thin film have been evaluated from absorption spectra. The direct energy band gap and Urbach energy of InSe thin film is found to be 1.90 eV and 235 meV respectively.

A new generation of x-ray spectrometry UHV instruments at the SR facilities BESSY II, ELETTRA and SOLEIL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lubeck, J., E-mail: janin.lubeck@ptb.de; Fliegauf, R.; Holfelder, I.

A novel type of ultra-high vacuum instrument for X-ray reflectometry and spectrometry-related techniques for nanoanalytics by means of synchrotron radiation (SR) has been constructed and commissioned at BESSY II. This versa-tile instrument was developed by the PTB, Germany’s national metrology institute, and includes a 9-axis manipulator that allows for an independent alignment of the samples with respect to all degrees of freedom. In addition, it integrates a rotational and translational movement of several photodiodes as well as a translational movement of a beam-geometry-defining aperture system. Thus, the new instrument enables various analytical techniques based on energy dispersive X-ray detectors suchmore » as reference-free X-Ray Fluorescence (XRF) analysis, total-reflection XRF, grazing-incidence XRF, in addition to optional X-Ray Reflectometry (XRR) measurements or polarization-dependent X-ray absorption fine structure analyses (XAFS). Samples having a size of up to (100 × 100) mm{sup 2}; can be analyzed with respect to their mass deposition, elemental, spatial or species composition. Surface contamination, nanolayer composition and thickness, depth pro-file of matrix elements or implants, nanoparticles or buried interfaces as well as molecular orientation of bonds can be accessed. Three technology transfer projects of adapted instruments have enhanced X-Ray Spectrometry (XRS) research activities within Europe at the synchrotron radiation facilities ELETTRA (IAEA) and SOLEIL (CEA/LNE-LNHB) as well as at the X-ray innovation laboratory BLiX (TU Berlin) where different laboratory sources are used. Here, smaller chamber requirements led PTB in cooperation with TU Berlin to develop a modified instrument equipped with a 7-axis manipulator: reduced freedom in the choice of experimental geometry modifications (absence of out-of-SR-plane and reference-free XRS options) has been compensated by encoder-enhanced angular accuracy for GIXRF and XRR.« less

Oxygen, Neon, and Iron X-Ray Absorption in the Local Interstellar Medium

NASA Technical Reports Server (NTRS)

Gatuzz, Efrain; Garcia, Javier; Kallman, Timothy R.; Mendoza, Claudio

2016-01-01

We present a detailed study of X-ray absorption in the local interstellar medium by analyzing the X-ray spectra of 24 galactic sources obtained with the Chandra High Energy Transmission Grating Spectrometer and the XMM-Newton Reflection Grating Spectrometer. Methods. By modeling the continuum with a simple broken power-law and by implementing the new ISMabs X-ray absorption model, we have estimated the total H, O, Ne, and Fe column densities towards the observed sources. Results. We have determined the absorbing material distribution as a function of source distance and galactic latitude longitude. Conclusions. Direct estimates of the fractions of neutrally, singly, and doubly ionized species of O, Ne, and Fe reveal the dominance of the cold component, thus indicating an overall low degree of ionization. Our results are expected to be sensitive to the model used to describe the continuum in all sources.

In-Line Phase-Contrast X-ray Imaging and Tomography for Materials Science

PubMed Central

Mayo, Sheridan C.; Stevenson, Andrew W.; Wilkins, Stephen W.

2012-01-01

X-ray phase-contrast imaging and tomography make use of the refraction of X-rays by the sample in image formation. This provides considerable additional information in the image compared to conventional X-ray imaging methods, which rely solely on X-ray absorption by the sample. Phase-contrast imaging highlights edges and internal boundaries of a sample and is thus complementary to absorption contrast, which is more sensitive to the bulk of the sample. Phase-contrast can also be used to image low-density materials, which do not absorb X-rays sufficiently to form a conventional X-ray image. In the context of materials science, X-ray phase-contrast imaging and tomography have particular value in the 2D and 3D characterization of low-density materials, the detection of cracks and voids and the analysis of composites and multiphase materials where the different components have similar X-ray attenuation coefficients. Here we review the use of phase-contrast imaging and tomography for a wide variety of materials science characterization problems using both synchrotron and laboratory sources and further demonstrate the particular benefits of phase contrast in the laboratory setting with a series of case studies. PMID:28817018

In-Line Phase-Contrast X-ray Imaging and Tomography for Materials Science.

PubMed

Mayo, Sheridan C; Stevenson, Andrew W; Wilkins, Stephen W

2012-05-24

X-ray phase-contrast imaging and tomography make use of the refraction of X-rays by the sample in image formation. This provides considerable additional information in the image compared to conventional X-ray imaging methods, which rely solely on X-ray absorption by the sample. Phase-contrast imaging highlights edges and internal boundaries of a sample and is thus complementary to absorption contrast, which is more sensitive to the bulk of the sample. Phase-contrast can also be used to image low-density materials, which do not absorb X-rays sufficiently to form a conventional X-ray image. In the context of materials science, X-ray phase-contrast imaging and tomography have particular value in the 2D and 3D characterization of low-density materials, the detection of cracks and voids and the analysis of composites and multiphase materials where the different components have similar X-ray attenuation coefficients. Here we review the use of phase-contrast imaging and tomography for a wide variety of materials science characterization problems using both synchrotron and laboratory sources and further demonstrate the particular benefits of phase contrast in the laboratory setting with a series of case studies.

Simulation of Near-Edge X-ray Absorption Fine Structure with Time-Dependent Equation-of-Motion Coupled-Cluster Theory.

PubMed

Nascimento, Daniel R; DePrince, A Eugene

2017-07-06

An explicitly time-dependent (TD) approach to equation-of-motion (EOM) coupled-cluster theory with single and double excitations (CCSD) is implemented for simulating near-edge X-ray absorption fine structure in molecular systems. The TD-EOM-CCSD absorption line shape function is given by the Fourier transform of the CCSD dipole autocorrelation function. We represent this transform by its Padé approximant, which provides converged spectra in much shorter simulation times than are required by the Fourier form. The result is a powerful framework for the blackbox simulation of broadband absorption spectra. K-edge X-ray absorption spectra for carbon, nitrogen, and oxygen in several small molecules are obtained from the real part of the absorption line shape function and are compared with experiment. The computed and experimentally obtained spectra are in good agreement; the mean unsigned error in the predicted peak positions is only 1.2 eV. We also explore the spectral signatures of protonation in these molecules.

Submicron hard X-ray fluorescence imaging of synthetic elements.

PubMed

Jensen, Mark P; Aryal, Baikuntha P; Gorman-Lewis, Drew; Paunesku, Tatjana; Lai, Barry; Vogt, Stefan; Woloschak, Gayle E

2012-04-13

Synchrotron-based X-ray fluorescence microscopy (XFM) using hard X-rays focused into sub-micron spots is a powerful technique for elemental quantification and mapping, as well as microspectroscopic measurements such as μ-XANES (X-ray absorption near edge structure). We have used XFM to image and simultaneously quantify the transuranic element plutonium at the L(3) or L(2)-edge as well as Th and lighter biologically essential elements in individual rat pheochromocytoma (PC12) cells after exposure to the long-lived plutonium isotope (242)Pu. Elemental maps demonstrate that plutonium localizes principally in the cytoplasm of the cells and avoids the cell nucleus, which is marked by the highest concentrations of phosphorus and zinc, under the conditions of our experiments. The minimum detection limit under typical acquisition conditions with an incident X-ray energy of 18 keV for an average 202 μm(2) cell is 1.4 fg Pu or 2.9×10(-20) moles Pu μm(-2), which is similar to the detection limit of K-edge XFM of transition metals at 10 keV. Copper electron microscopy grids were used to avoid interference from gold X-ray emissions, but traces of strontium present in naturally occurring calcium can still interfere with plutonium detection using its L(α) X-ray emission. Copyright © 2012 Elsevier B.V. All rights reserved.

Sub-micron Hard X-ray Fluorescence Imaging of Synthetic Elements

PubMed Central

Jensen, Mark P.; Aryal, Baikuntha P.; Gorman-Lewis, Drew; Paunesku, Tatjana; Lai, Barry; Vogt, Stefan; Woloschak, Gayle E.

2013-01-01

Synchrotron-based X-ray fluorescence microscopy (SXFM) using hard X-rays focused into sub-micron spots is a powerful technique for elemental quantification and mapping, as well as microspectroscopic measurement such as μ-XANES (X-ray absorption near edge structure). We have used SXFM to image and simultaneously quantify the transuranic element plutonium at the L3 or L2 edge as well as lighter biologically essential elements in individual rat pheochromocytoma (PC12) cells after exposure to the long-lived plutonium isotope 242Pu. Elemental maps reveal that plutonium localizes principally in the cytoplasm of the cells and avoids the cell nucleus, which is marked by the highest concentrations of phosphorus and zinc, under the conditions of our experiments. The minimum detection limit under typical acquisition conditions for an average 202 μm2 cell is 1.4 fg Pu/cell or 2.9 × 10−20 moles Pu/μm2, which is similar to the detection limit of K-edge SXFM of transition metals at 10 keV. Copper electron microscopy grids were used to avoid interference from gold X-ray emissions, but traces of strontium present in naturally occurring calcium can still interfere with plutonium detection using its Lα X-ray emission. PMID:22444530

Crystal growth, structural, thermal and mechanical behavior of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) single crystals.

PubMed

Mahadevan, M; Ramachandran, K; Anandan, P; Arivanandhan, M; Bhagavannarayana, G; Hayakawa, Y

2014-12-10

Single crystals of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) have been grown successfully from the solution of l-arginine and 4-nitrophenol. Slow evaporation of solvent technique was adopted to grow the bulk single crystals. Single crystal X-ray diffraction analysis confirms the grown crystal has monoclinic crystal system with space group of P21. Powder X-ray diffraction analysis shows the good crystalline nature. The crystalline perfection of the grown single crystals was analyzed by HRXRD by employing a multicrystal X-ray diffractometer. The functional groups were identified from proton NMR spectroscopic analysis. Linear and nonlinear optical properties were determined by UV-Vis spectrophotometer and Kurtz powder technique respectively. It is found that the grown crystal has no absorption in the green wavelength region and the SHG efficiency was found to be 2.66 times that of the standard KDP. The Thermal stability of the crystal was found by obtaining TG/DTA curve. The mechanical behavior of the grown crystal has been studied by Vicker's microhardness method. Copyright © 2014 Elsevier B.V. All rights reserved.