Sample records for electron microprobe x-ray

  1. Electron microprobe mineral analysis guide

    NASA Technical Reports Server (NTRS)

    Brown, R. W.

    1980-01-01

    Electron microprobe mineral analysis guide is a compilation of X-ray tables and spectra recorded from various mineral matrices. Spectra were obtained using electron microprobe, equipped with LiF geared, curved crystal X-ray spectrometers, utilizing typical analytical operating conditions: 15 Kv acceleration potential, 0.02 microampere sample current as measured on a clinopyroxene standard (CP19). Tables and spectra are presented for the majority of elements, fluorine through uranium, occurring in mineral samples from lunar, meteoritic and terrestrial sources. Tables for each element contain relevant analytical information, i.e., analyzing crystal, X-ray peak, background and relative intensity information, X-ray interferences and a section containing notes on the measurement. Originally intended to cover silicates and oxide minerals the tables and spectra have been expanded to cover other mineral phases. Electron microprobe mineral analysis guide is intended as a spectral base to which additional spectra can be added as the analyst encounters new mineral matrices.

  2. 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.

  3. 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.

  4. Wavelength dispersive analysis with the synchrotron x ray fluorescence microprobe

    NASA Technical Reports Server (NTRS)

    Rivers, M. L.; Thorn, K. S.; Sutton, S. R.; Jones, K. W.; Bajt, S.

    1993-01-01

    A wavelength dispersive spectrometer (WDS) was tested on the synchrotron x ray fluorescence microprobe at Brookhaven National Laboratory. Compared to WDS spectra using an electron microprobe, the synchrotron WDS spectra have much better sensitivity and, due to the absence of bremsstrahlung radiation, lower backgrounds. The WDS spectrometer was successfully used to resolve REE L fluorescence spectra from standard glasses and transition metal K fluorescence spectra from kamacite.

  5. Recent advances in X-ray microanalysis in dermatology

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

    Forslind, B.; Grundin, T.G.; Lindberg, M.

    1985-01-01

    Electron microprobe and proton microprobe X-ray analysis can be used in several areas of dermatological research. With a proton probe, the distribution of trace elements in human hair can be determined. Electron microprobe analysis on freeze-dried cryosections of guinea-pig and human epidermis shows a marked gradient of Na, P and K over the stratum granulosum. In sections of freeze-substituted human skin this gradient is less steep. This difference is likely to be due to a decrease in water content of the epidermis towards the stratum corneum. Electron microprobe analysis of the epidermis can, for analysis of trace elements, be complementedmore » by the proton microprobe. Quantitative agreement between the two techniques can be obtained by the use of a standard. Proton microprobe analysis was used to determine the distribution of Ni or Cr in human epidermis exposed to nickel or chromate ions. Possible differences in water content between the stratum corneum of patients with atopic eczema and normal stratum corneum was investigated in skin freeze-substituted with Br-doped resin. No significant differences were observed.« less

  6. Age mapping and dating of monazite on the electron microprobe: Deconvoluting multistage tectonic histories

    NASA Astrophysics Data System (ADS)

    Williams, Michael L.; Jercinovic, Michael J.; Terry, Michael P.

    1999-11-01

    High-resolution X-ray mapping and dating of monazite on the electron microprobe are powerful geochronological tools for structural, metamorphic, and tectonic analysis. X-ray maps commonly show complex Th, U, and Pb zoning that reflects monazite growth and overgrowth events. Age maps constructed from the X-ray maps simplify the zoning and highlight age domains. Microprobe dating offers a rapid, in situ method for estimating ages of mapped domains. Application of these techniques has placed new constraints on the tectonic history of three areas. In western Canada, age mapping has revealed multiphase monazite, with older cores and younger rims, included in syntectonic garnet. Microprobe ages show that tectonism occurred ca. 1.9 Ga, 700 m.y. later than mylonitization in the adjacent Snowbird tectonic zone. In New Mexico, age mapping and dating show that the dominant fabric and triple-point metamorphism occurred during a 1.4 Ga reactivation, not during the 1.7 Ga Yavapai-Mazatzal orogeny. In Norway, monazite inclusions in garnet constrain high-pressure metamorphism to ca. 405 Ma, and older cores indicate a previously unrecognized component of ca. 1.0 Ga monazite. In all three areas, microprobe dating and age mapping have provided a critical textural context for geochronologic data and a better understanding of the complex age spectra of these multistage orogenic belts.

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

    Ice, G.E.; Barbee, T.; Bionta, R.

    The increasing availability of synchrotron x-ray sources has stimulated the development of advanced hard x-ray (E{>=}5 keV) microprobes. New x-ray optics have been demonstrated which show promise for achieving intense submicron hard x-ray probes. These probes will be used for extraordinary elemental detection by x-ray fluorescence/absorption and for microdiffraction to identify phase and strain. The inherent elemental and crystallographic sensitivity of an x-ray microprobe and its inherently nondestructive and penetrating nature makes the development of an advanced hard x-ray microprobe an important national goal. In this workshop state-of-the-art hard x-ray microprobe optics were described and future directions were discussed. Genemore » Ice, Oak Ridge National Laboratory (ORNL), presented an overview of the current status of hard x-ray microprobe optics and described the use of crystal spectrometers to improve minimum detectable limits in fluorescent microprobe experiments. Al Thompson, Lawrence Berkeley Laboratory (LBL), described work at the Center for X-ray Optics to develop a hard x-ray microprobe based on Kirkpatrick-Baez (KB) optics. Al Thompson also showed the results of some experimental measurements with their KB optics. Malcolm Howells presented a method for bending elliptical mirrors and Troy Barbee commented on the use of graded d spacings to achieve highest efficiency in KB multilayer microfocusing. Richard Bionta, Lawrence Livermore National Laboratory (LLNL), described the development of the first hard x-ray zone plates and future promise of so called {open_quotes}jelly roll{close_quotes} or sputter slice zone plates. Wenbing Yun, Argonne National Laboratory (ANL), described characterization of jelly roll and lithographically produced zone plates and described the application of zone plates to focus extremely narrow bandwidths by nuclear resonance. This report summarizes the presentations of the workshop subgroup on hard x-ray microprobes.« less

  8. Investigation of Synthetic Mg(1.3)V(1.7)O4 Spinel with MgO Inclusions: Case Study of a Spinel with an Apparently occupied Interstitial Site

    NASA Technical Reports Server (NTRS)

    Uchida, Hinako; Righter, Kevin; Lavina, Barbara; Nowell, Matthew M.; Wright, Stuart I.; Downs, Robert T.; Yang, Hexiong

    2007-01-01

    A magnesium vanadate spinel crystal, ideally MgV2O4, synthesized at 1 bar, 1200 C and equilibrated under FMQ + 1.3 log f(sub o2) condition, was investigated using single-crystal X-ray diffraction, electron microprobe, and electron backscatter (EBSD). The initial X-ray structure refinements gave tetrahedral and octahedral site occupancies, along with the presence of 0.053 apfu Mg at an interstitial octahedral site . Back-scattered electron (BSE) images and electron microprobe analyses revealed the existence of an Mg-rich phase in the spinel matrix, which was too small (less than or equal to 3microns) for an accurate chemical determination. The EBSD analysis combined with X-ray energy dispersive spectroscop[y (XEDS) suggested that the Mg-rich inclusions are periclase oriented coherently with the spinel matrix. The final structure refinements were optimized by subtracting the X-ray intensity contributions (approx. 9%) of periclase reflections, which eliminated the interstitial Mg. This study provides insight into possible origins of refined interstitial cations reported in the the literature for spinel, and points to the difficulty of using only X-ray diffraction data to distinguish a spinel with interstitial cations from one with coherently oriented MgO inclusions.

  9. The electron microprobe as a metallographic tool

    NASA Technical Reports Server (NTRS)

    Goldstein, J. I.

    1974-01-01

    The electron microprobe (EMP) is shown to represent one of the most powerful techniques for the examination of the microstructure of materials. It is an electron optical instrument in which compositional and topographic information is obtained from regions smaller than 1 micron in diameter on a specimen. Photographs of compositional and topographic changes in 1-sq-mm to 20-sq-micron areas on various types of specimens can also be obtained. These photographs are strikingly similar to optical photomicrographs. Various signals measured in the EMP (X-rays, secondary electrons, backscattered electrons, etc.) are discussed, along with their resolution and the type of information they may help obtain. In addition to elemental analysis, solid state detecting and scanning techniques are reviewed. Various techniques extending the EMP instrument capabilities, such as deconvolution and soft X-ray analysis, are also described.

  10. Electron microprobe analysis program for biological specimens: BIOMAP

    NASA Technical Reports Server (NTRS)

    Edwards, B. F.

    1972-01-01

    BIOMAP is a Univac 1108 compatible program which facilitates the electron probe microanalysis of biological specimens. Input data are X-ray intensity data from biological samples, the X-ray intensity and composition data from a standard sample and the electron probe operating parameters. Outputs are estimates of the weight percentages of the analyzed elements, the distribution of these estimates for sets of red blood cells and the probabilities for correlation between elemental concentrations. An optional feature statistically estimates the X-ray intensity and residual background of a principal standard relative to a series of standards.

  11. Ilmenite exsolution schemes in Apollo-17 high-Ti basalts

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

    Vaniman, D.; Heiken, G.; Muhich, T.

    1990-01-01

    Combined electron microprobe and scanning electron microscope (SEM) x-ray image analyses are used to obtain semiquantitative data on the relations between ilmenite grains and their exsolved chromite and rutile. Comparisons of these data for ilmenites in four Apollo-17 high-Ti basalts with a database of electron microprobe analyses from the literature indicates that Cr expulsion from ilmenite can be as important as Fe{sup 2+} reduction in causing subsolidus exsolution of chromite and rutile from ilmenite. 12 refs., 4 figs., 5 tabs.

  12. The Perils of Electron Microprobe Analysis of Apatite

    NASA Astrophysics Data System (ADS)

    Henderson, C. E.; Essene, E. J.; Wang, K. L.; Zhang, Y.

    2010-12-01

    Accurate electron microprobe analysis of apatite is problematic, especially for F and Cl, whose concentrations are essential in calculating a non-analyzable OH component. The issues include beam-induced sample damage and temporal variation of F and Cl X-rays; both effects are mainly dependent on beam current, beam spot size and apatite orientation [1]. To establish a rigorous analytical procedure, several oriented apatite samples, including the well-known Durango and Wilberforce fluorapatites, were analyzed for a large suite of elements, including oxygen. Careful X-ray spectroscopy was performed, including selection of appropriate analytical standards, background measurement positions and comparison of area peak factors. Polarized infrared spectra on oriented apatite samples were also collected for complementary information. The results show that when apatite samples are oriented with the c-axis parallel to the electron beam, there is significant nonlinear variation (an increase or decrease, depending on measurement conditions) of F and Cl X-ray intensities during analyses, and systematically higher-than-expected F apparent concentrations, despite the careful selection of electron beam conditions from a series of X-ray time scans and zero-time count rate extrapolation. On the other hand, when the electron beam is oriented perpendicular to the c-axis, with a ≤ 15 nA beam current and a ≥ 5 µm diameter defocused beam, F and Cl X-ray intensities do not vary or vary slowly and predictably with time, yielding quantitative analysis results for the Durango and Wilberforce apatites (both containing little OH) which are in good agreement with published wet chemical analyses. Furthermore, the OH and CO2 contents inferred for three other analyzed apatite samples are roughly consistent with infrared analyses. For example, for an apatite from Silver Crater Mine in Ontario, significant deficiency in the P site, as well as extra F, was inferred from microprobe analyses. Infrared spectra show a strong band of (CO3)2- for this apatite, which indicates a possible substitution of (CO3)2-(F)- for (PO4)3-. Other techniques to mitigate temporal variation of F and Cl, including alternative metal coatings, concurrent stage movement, and cryogenic sample-cooling were attempted, but did not eliminate the disparity in measured F concentrations between the two sample orientations. Thus, we believe that F measurements on F-rich apatite samples of unknown orientation are immediately suspect and should be regarded as upper limits of true F concentration. X-ray mapping, CL imaging and subsequent quantitative analyses show compositional variations in Na, S, Si, and REE in the Durango and Wilberforce fluorapatite samples used in this study. Problems of electron beam sensitivity, X-ray intensity anisotropy due to sample orientation, and compositional heterogeneity call into question their continued use as routine microanalysis reference materials. Microanalysts are encouraged to use more robust calibration standards, such as Cl-rich or other F-poor apatites for Ca, P, O and Cl, and MgF2 for F measurements. [1] Stormer, J.C., Pierson, M.L, and Tacker, R.C. (1993) Variation of F and Cl X-ray intensity due to anisotropic diffusion in apatite during electron microprobe analysis. Am. Min., 78, 641-648.

  13. Use of scanning electron microscopy and microanalysis to determine chloride content of concrete and raw materials.

    DOT National Transportation Integrated Search

    2013-02-01

    Standard sample sets of cement and mortar formulations with known levels of Cl as well as concrete samples subject to Cl diffusion were all prepared for and analyzed with scanning electron microscopy (SEM) and electron microprobe (EPMA). Using x-ray ...

  14. Clusters of Defects in Semiconductors

    DTIC Science & Technology

    1984-08-01

    onecionbewen-te heica seces .-. o* Fe and.th deec prd *n th *Rlmnecne ae t..* E. STATISTICS The funds from this contract were used to support the research of...characterized at Hughes Research Laboratories. L x No Np N1 . Electron X-ray Sample (cm- 1) (cm- ) (cm-3 ) microprobe Density diffraction .. -. C077 3.6x 10

  15. Probing molecular dynamics in solution with x-ray valence-to-core spectroscopy

    NASA Astrophysics Data System (ADS)

    Doumy, Gilles; March, Anne Marie; Tu, Ming-Feng; Al Haddad, Andre; Southworth, Stephen; Young, Linda; Walko, Donald; Bostedt, Christoph

    2017-04-01

    Hard X-ray spectroscopies are powerful tools for probing the electronic and geometric structure of molecules in complex or disordered systems and have been particularly useful for studying molecules in the solution phase. They are element specific, sensitive to the electronic structure and the local arrangements of surrounding atoms of the element being selectively probed. When combined in a pump-probe scheme with ultrafast lasers, X-ray spectroscopies can be used to track the evolution of structural changes that occur after photoexcitation. Efficient use of hard x-ray radiation coming from high brilliance synchrotrons and upcoming high repetition rate X-ray Free Electron Lasers requires MHz repetition rate lasers and data acquisition systems. High information content Valence-to-Core x-ray emission is directly sensitive to the molecular orbitals involved in photochemistry. We report on recent progress towards fully enabling this photon-hungry technique for the study of time-resolved molecular dynamics, including efficient detection and use of polychromatic x-ray micro-probe at the Advanced Photon Source. Work was supported by the U.S. Department of Energy, Office of Science, Chemical Sciences, Geosciences, and Biosciences Division.

  16. PROTON MICROPROBE ANALYSIS OF TRACE-ELEMENT VARIATIONS IN VITRINITES IN THE SAME AND DIFFERENT COAL BEDS.

    USGS Publications Warehouse

    Minkin, J.A.; Chao, E.C.T.; Blank, Herma; Dulong, F.T.

    1987-01-01

    The PIXE (proton-induced X-ray emission) microprobe can be used for nondestructive, in-situ analyses of areas as small as those analyzed by the electron microprobe, and has a sensitivity of detection as much as two orders of magnitude better than the electron microprobe. Preliminary studies demonstrated that PIXE provides a capability for quantitative determination of elemental concentrations in individual coal maceral grains with a detection limit of 1-10 ppm for most elements analyzed. Encouraged by the earlier results, we carried out the analyses reported below to examine trace element variations laterally (over a km range) as well as vertically (cm to m) in the I and J coal beds in the Upper Cretaceous Ferron Sandstone Member of the Mancos Shale in central Utah, and to compare the data with the data from two samples of eastern coals of Pennsylvanian age.

  17. Micro Electron MicroProbe and Sample Analyzer

    NASA Technical Reports Server (NTRS)

    Manohara, Harish; Bearman, Gregory; Douglas, Susanne; Bronikowski, Michael; Urgiles, Eduardo; Kowalczyk, Robert; Bryson, Charles

    2009-01-01

    A proposed, low-power, backpack-sized instrument, denoted the micro electron microprobe and sample analyzer (MEMSA), would serve as a means of rapidly performing high-resolution microscopy and energy-dispersive x-ray spectroscopy (EDX) of soil, dust, and rock particles in the field. The MEMSA would be similar to an environmental scanning electron microscope (ESEM) but would be much smaller and designed specifically for field use in studying effects of geological alteration at the micrometer scale. Like an ESEM, the MEMSA could be used to examine uncoated, electrically nonconductive specimens. In addition to the difference in size, other significant differences between the MEMSA and an ESEM lie in the mode of scanning and the nature of the electron source.

  18. XAP, a program for deconvolution and analysis of complex X-ray spectra

    USGS Publications Warehouse

    Quick, James E.; Haleby, Abdul Malik

    1989-01-01

    The X-ray analysis program (XAP) is a spectral-deconvolution program written in BASIC and specifically designed to analyze complex spectra produced by energy-dispersive X-ray analytical systems (EDS). XAP compensates for spectrometer drift, utilizes digital filtering to remove background from spectra, and solves for element abundances by least-squares, multiple-regression analysis. Rather than base analyses on only a few channels, broad spectral regions of a sample are reconstructed from standard reference spectra. The effects of this approach are (1) elimination of tedious spectrometer adjustments, (2) removal of background independent of sample composition, and (3) automatic correction for peak overlaps. Although the program was written specifically to operate a KEVEX 7000 X-ray fluorescence analytical system, it could be adapted (with minor modifications) to analyze spectra produced by scanning electron microscopes, electron microprobes, and probes, and X-ray defractometer patterns obtained from whole-rock powders.

  19. Doubly curved mica diffractors and their applications to x-ray microprobe fluorescence and microanalysis

    NASA Astrophysics Data System (ADS)

    Chen, Zewu

    This thesis describes the experimental work in the fabrication of doubly-curved mica diffractors and their applications in monochromatic microprobe x-ray fluorescence analysis and wavelength dispersive spectrometry. Three-dimension focusing of x-rays can be achieved by diffraction from a doubly-curved diffractor. A Johann point-focusing mica diffractor was fabricated for focusing the Cu Kα1 radiation and characterized by using a microfocus x-ray source. The intensity of the focused beam was measured to be 1.01 × 108 photons/s at the focal spot. The spot size of the focused beam was measured by the knife edge scan method. A Cu Kα1 focal spot of 43 μm x 68 μm has been obtained. Monochromatic microprobe x-ray fluorescence (MMXRF) analysis was performed by using the focused Cu Kα1 radiation. The microfocus x-ray source was operated at 30 kV and 0.1 mA. MMXRF spectra of bulk specimens of GaAs, Si, ZnSe, Mg and 40 μm thick Muscovite were recorded with a Si(Li) energy dispersive detector. Exceptional high signal-to-background ratios were observed. Due to the low background, detection limits as low as 1.6 ppm were predicted for a measurement time of 500 s for bulk specimens. The detector background was determined by recording a spectrum from an Fe55 source and was found to be a significant contribution to the total observed background. A wavelength dispersive spectrometer was designed and constructed for the use in a JEOL transmission electron microscope. A logarithmic spiral of revolution diffractor was fabricated and used explored for measurement of Ca concentration in the TEM. Bench tests were carried out by using the microfocus x-ray source. Preliminary data of tests in the TEM indicated that the spectrometer may give better performance than EDS systems previously used.

  20. The detection of sulphur in contamination spots in electron probe X-ray microanalysis

    USGS Publications Warehouse

    Adler, I.; Dwornik, E.J.; Rose, H.J.

    1962-01-01

    Sulphur has been identified as one of the elements present in the contamination spot which forms under the electron beam in the microprobe. The presence of the sulphur results in a rapid change in intensity measurements causing a loss of observed intensity for elements other than sulphur. The source of sulphur has been traced at least in part to the Apiezon B diffusion pump oil. A comparative X-ray fluorescence study of the Apiezon B and Octoil diffusion pump oils showed substantial amounts of sulphur in the Apiezon B. The Octoil was relatively free of sulphur.

  1. Hot Corrosion Degradation of Metals and Alloys - A Unified Theory

    DTIC Science & Technology

    1979-06-01

    microscope, electron beam microprobe and X-ray diffraction. REULTS AND DMCtESION Hot Corrosion Degradation Sectuence In attempting to develop a unified...Figure 40a. Such ghost images, which can be called corrosion front ghosts , appear as sequential dark and light zones in electron backscatter images... Electronic and Solid State Sciences AUG Ill 1979I Bolling AFB, D.C. 20332 ID PRATT &WHITNEY ARCRAFT GROUP P.O . Box 2861 /Government Products Division wi

  2. Synchrotron X-ray microscopy and spectroscopy analysis of iron in hemochromatosis liver and intestines

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

    Ko, J .Y. Peter; Sham, Tsun-Kong; Chakrabarti, Subrata

    2009-12-01

    Hemochromatosis is a genetic disorder that causes body to store excess iron in organs such as heart or liver. Distribution of iron, as well as copper, zinc and calcium, and chemical identity of iron in hemochromatosis liver and intestine were investigated by X-ray microprobe experiments, which consist of X-ray microscopy and micro-X-ray absorption fine structure. Our results show that iron concentration in hemochromatosis liver tissue is high, while much less Fe is found in intestinal tissue. Moreover, chemical identity of Fe in hemochromatosis liver can be identified. X-ray microprobe experiments allows for examining elemental distribution at an excellent spatial resolution.more » Moreover, chemical identity of element of interest can be obtained.« less

  3. Spatial investigation of some uranium minerals using nuclear microprobe

    NASA Astrophysics Data System (ADS)

    Valter, Anton A.; Knight, Kim B.; Eremenko, Gelij K.; Magilin, Dmitry V.; Ponomarov, Artem A.; Pisansky, Anatoly I.; Romanenko, Alexander V.; Ponomarev, Alexander G.

    2018-01-01

    In this work, several individual grains of uranium minerals—uraninite with high content of Ca, Ca-rich boltwoodite, growths of uranophane with β-uranophane, and weeksite—from different uranium deposits were studied by a scanning nuclear microprobe. Particle-induced X-ray emission technique provided by the microprobe (µ-PIXE) was carried out to obtain a concentration and 2D distribution of elements in these minerals. In addition, energy dispersive X-ray spectrometry (SEM-EDS) provided by a scanning electron microscope was used. The types of minerals were determined by X-ray diffraction methods. Results of this study improved the understanding of trace elemental composition of the uranium minerals depending on their origin. Obtained signatures could be linked then to the sample provenance. Such data are important for nuclear forensics to identify the ore types and even specific ore bodies, when only small samples may be available for analysis. In this study, the µ-PIXE technique was used for obtaining the 2D distribution of trace elements that are not commonly measured by SEM-EDS at the relevant concentrations. The detected levels and precisions of elements determination by µ-PIXE were also defined. Using µ-PIXE, several micro mineral inclusions such as phosphate with high level of V and Si were identified. The age of the uranium minerals was estimated due to a significant content of radiogenic Pb that provides an additional parameter for determination of the main attributive characteristics of the minerals. This work also showed that due to its high elemental sensitivity the nuclear microprobe can be a new analytical tool for creating a nuclear forensic database from the known uranium deposits and a subsequent analysis of the intercepted illicit materials.

  4. Spatial investigation of some uranium minerals using nuclear microprobe

    NASA Astrophysics Data System (ADS)

    Valter, Anton A.; Knight, Kim B.; Eremenko, Gelij K.; Magilin, Dmitry V.; Ponomarov, Artem A.; Pisansky, Anatoly I.; Romanenko, Alexander V.; Ponomarev, Alexander G.

    2018-06-01

    In this work, several individual grains of uranium minerals—uraninite with high content of Ca, Ca-rich boltwoodite, growths of uranophane with β-uranophane, and weeksite—from different uranium deposits were studied by a scanning nuclear microprobe. Particle-induced X-ray emission technique provided by the microprobe (µ-PIXE) was carried out to obtain a concentration and 2D distribution of elements in these minerals. In addition, energy dispersive X-ray spectrometry (SEM-EDS) provided by a scanning electron microscope was used. The types of minerals were determined by X-ray diffraction methods. Results of this study improved the understanding of trace elemental composition of the uranium minerals depending on their origin. Obtained signatures could be linked then to the sample provenance. Such data are important for nuclear forensics to identify the ore types and even specific ore bodies, when only small samples may be available for analysis. In this study, the µ-PIXE technique was used for obtaining the 2D distribution of trace elements that are not commonly measured by SEM-EDS at the relevant concentrations. The detected levels and precisions of elements determination by µ-PIXE were also defined. Using µ-PIXE, several micro mineral inclusions such as phosphate with high level of V and Si were identified. The age of the uranium minerals was estimated due to a significant content of radiogenic Pb that provides an additional parameter for determination of the main attributive characteristics of the minerals. This work also showed that due to its high elemental sensitivity the nuclear microprobe can be a new analytical tool for creating a nuclear forensic database from the known uranium deposits and a subsequent analysis of the intercepted illicit materials.

  5. ORIGIN OF QUARTZ IN COAL.

    USGS Publications Warehouse

    Ruppert, Leslie F.; Cecil, C. Blaine; Stanton, Ronald W.

    1984-01-01

    Both a scanning electron microscope and an electron microprobe (EMP) were used in this study to analyze the cathodoluminescence properties of quartz grains in samples of the Upper Freeport coal bed because quartz grains in coal are small (silt sized) and below the resolution capabilities of a standard luminoscope. Quartz grains were identified by the detection of silicon alone with energy dispersive X-ray units attached to both the SEM and the EMP.

  6. Scanning electron microscopy, x-ray diffraction, and electron microprobe analysis of calcific deposits on intrauterine contraceptive devices

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

    Khan, S.R.; Wilkinson, E.J.

    Deposits found on intrauterine contraceptive devices (IUDs) were studied by scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray microanalysis. All seven devices, including five plastic and two copper IUDs, were coated with a crust containing cellular, acellular, and fibrillar material. The cellular material was composed of erythrocytes, leukocytes, cells of epithelial origin, sperm, and bacteria. Some of the bacteria were filamentous, with acute-angle branching. The fibrillar material appeared to be fibrin. Most of the acellular material was amorphous; calcite was identified by x-ray diffraction, and x-ray microanalysis showed only calcium. Some of the acellular material, particularly that on themore » IUD side of the crust, was organized in spherulitic crystals and was identified as calcium phosphate by x-ray microanalysis. The crust was joined to the IUD surface by a layer of fibrillar and amorphous material. It is suggested that the initial event in the formation of calcific deposits on IUD surfaces is the deposition of an amorphous and fibrillar layer. Various types of cells present in the endometrial environment adhere to this layer and then calcify. Thus, the deposition of calcific material on the IUDs is a calcification phenomenon, not unlike the formation of plaque on teeth.« less

  7. Quantitative simultaneous multi-element microprobe analysis using combined wavelength and energy dispersive systems

    NASA Technical Reports Server (NTRS)

    Walter, L. S.; Doan, A. S., Jr.; Wood, F. M., Jr.; Bredekamp, J. H.

    1972-01-01

    A combined WDS-EDS system obviates the severe X-ray peak overlap problems encountered with Na, Mg, Al and Si common to pure EDS systems. By application of easily measured empirical correction factors for pulse pile-up and peak overlaps which are normally observed in the analysis of silicate minerals, the accuracy of analysis is comparable with that expected for WDS electron microprobe analyses. The continuum backgrounds are subtracted for the spectra by a spline fitting technique based on integrated intensities between the peaks. The preprocessed data are then reduced to chemical analyses by existing data reduction programs.

  8. Corrosion phenomena in electron, proton and synchrotron X-ray microprobe analysis of Roman glass from Qumran, Jordan

    NASA Astrophysics Data System (ADS)

    Janssens, K.; Aerts, A.; Vincze, L.; Adams, F.; Yang, C.; Utui, R.; Malmqvist, K.; Jones, K. W.; Radtke, M.; Garbe, S.; Lechtenberg, F.; Knöchel, A.; Wouters, H.

    1996-04-01

    A series of 89 glass fragments of Roman glass are studied using electron, proton and synchrotron radiation induced X-ray emission from microscopic areas on the sample surface. The glass originates from Qumran, Jordan and was buried for 1900 years. The weathering layers that result from the extended contact with ground water have been studied, next to the trace composition of the original glass of these pieces. The latter information indicates that at Qumran, large quantities of glass objects were being used in Ancient times. Cross-sectional profiles of the glass show a complex migration behaviour of various groups of major and trace elements.

  9. Magnetic particles extracted from manganese nodules: Suggested origin from stony and iron meteorites

    USGS Publications Warehouse

    Finkelman, R.B.

    1970-01-01

    On the basis of x-ray diffraction and electron microprobe data, spherical and ellipsoidal particles extracted from manganese nodules were divided into three groups. Group I particles are believed to be derived from iron meteorites, and Group II particles from stony meteorites. Group III particles are believed to be volcanic in origin.

  10. Preliminary study on the mode of occurrence of arsenic in high arsenic coals from southwest Guizhou Province

    USGS Publications Warehouse

    Ding, Z.; Zheng, B.; Zhang, Jiahua; Belkin, H.E.; Finkelman, R.B.; Zhao, F.; Zhou, D.; Zhou, Y.; Chen, C.

    1999-01-01

    Coal samples from high arsenic coal areas have been analyzed by electron microprobe analyzer (EMPA), scanning electron microscopy with an energy dispersive X-ray analyzer (SEM-EDX), X-ray diffraction analysis (XRD), low temperature ashing (LTA), transmission electron microscopy (TEM), X-ray absorption fine structure (XAFS), instrument neutron activation analysis (INAA) and wet chemical analysis. Although some As-bearing minerals such as pyrite, arsenopyrite, realgar (?), As-bearing sulfate, and As-bearing clays are found in the high arsenic coals, their contents do not account for the abundance of arsenic in the some coals. Analysis of the coal indicates that arsenic exists mainly in the form of As5+ and As3+, combined with compounds in the organic matrix. The occurrence of such exceptionally high arsenic contents in coal and the fact that the arsenic is dominantly organically associated are unique observations. The modes of occurrence of arsenic in high As-coals are discussed.

  11. Sulfur speciation in hydrous experimental glasses of varying oxidation state - Results from measured wavelength shifts of sulfur X-rays

    NASA Technical Reports Server (NTRS)

    Carroll, Michael R.; Rutherford, Malcolm J.

    1988-01-01

    The focusing geometry of an electron microprobe has been used to measure the wavelength shifts of sulfur X-rays from hydrous experimental melts synthesized at oxygen fugacities that range from near the iron-wustite buffer to the magnetite-hermatite buffer. It is found that the proportion of dissolved sulfur which is present as sulfate increases with increasing oxygen fugacity. It is noted that in natural melts that have equilibrated at or below fayalite-magnetite-quartz values of +1, sulfur is probably present mainly as S(2-).

  12. Trace elemental analysis of bituminuos coals using the Heidelberg proton microprobe

    USGS Publications Warehouse

    Chen, J.R.; Kneis, H.; Martin, B.; Nobiling, R.; Traxel, K.; Chao, E.C.T.; Minkin, J.A.

    1981-01-01

    Trace elements in coal can occur as components of either the organic constituents (macerals) or the inorganic constituents (minerals). Studies of the concentrations and distribution of the trace elements are vital to understanding the geochemical millieu in which the coal was formed and in evaluating the attempts to recover rare but technologically valuable metals. In addition, information on the trace element concentrations is important in predicting the environmental impact of burning particular coals, as many countries move toward greater utilization of coal reserves for energy production. Traditionally, the optical and the electron microscopes and more recently the electron microprobe have been used in studying the components of coal. The proton-induced X-ray emission (PIXE) microprobe offers a new complementary approach with an order of magnitude or more better minimum detection limit. We present the first measurements with a PIXE microprobe of the trace element concentrations of bituminous coal samples. Elemental analyses of the coal macerals-vitrinite, exinite, and inertinite-are discussed for three coal samples from the Eastern U.S.A., three samples from the Western U.S.A., and one sample from the Peoples Republic of China. ?? 1981.

  13. Effect of Cooling Rates on γ → α Transformation and Metastable States in Fe-Cu Alloys with Addition of Ni

    NASA Astrophysics Data System (ADS)

    Crozet, C.; Verdier, M.; Lay, S.; Antoni-Zdziobek, A.

    2018-07-01

    α/γ phase transformations occurring in Fe-10Cu-xNi alloys (0 ≤ x ≤ 15 in mass%) were studied using X-ray diffraction, scanning electron microscopy, electron back scattered diffraction, transmission electron microscopy and chemical analysis, combining X-ray microanalysis with energy dispersive spectrometry in the scanning electron microscope and electron microprobe analysis with wavelength dispersive spectrometry. The influence of cooling rate on the microstructure was investigated using ice-brine quenching and 2 °C/min slow cooling rate performed with dilatometry. Ni addition induces metastable transformations on cooling: massive and bainitic ferrite are formed depending on the alloy composition and cooling rate. Moreover, most of the Cu phase precipitates on cooling giving rise to a fine distribution of Cu particles in the ferrite grains. For both cooling conditions, the hardness increases with increasing Ni content and a higher hardness is obtained in the quenched alloy for each composition. The change in hardness is correlated to the effect of Ni solid solution, transformation structure and size of Cu particles.

  14. X-ray microprobe of orbital alignment in strong-field ionized atoms.

    PubMed

    Young, L; Arms, D A; Dufresne, E M; Dunford, R W; Ederer, D L; Höhr, C; Kanter, E P; Krässig, B; Landahl, E C; Peterson, E R; Rudati, J; Santra, R; Southworth, S H

    2006-08-25

    We have developed a synchrotron-based, time-resolved x-ray microprobe to investigate optical strong-field processes at intermediate intensities (10(14) - 10(15) W/cm2). This quantum-state specific probe has enabled the direct observation of orbital alignment in the residual ion produced by strong-field ionization of krypton atoms via resonant, polarized x-ray absorption. We found strong alignment to persist for a period long compared to the spin-orbit coupling time scale (6.2 fs). The observed degree of alignment can be explained by models that incorporate spin-orbit coupling. The methodology is applicable to a wide range of problems.

  15. Non-destructive trace element microanalysis of as-received cometary nucleus samples using synchrotron x ray fluorescence

    NASA Technical Reports Server (NTRS)

    Sutton, S. R.

    1989-01-01

    The Synchrotron X ray Fluorescence (SXRF) microprobe at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory, will be an excellent instrument for non-destructive trace element analyses of cometary nucleus samples. Trace element analyses of as-received cometary nucleus material will also be possible with this technique. Bulk analysis of relatively volatile elements will be important in establishing comet formation conditions. However, as demonstrated for meteorites, microanalyses of individual phases in their petrographic context are crucial in defining the histories of particular components in unequilibrated specimens. Perhaps most informative in comparing cometary material with meteorites will be the halogens and trace metals. In-situ, high spatial resolution microanalyses will be essential in establishing host phases for these elements and identifying terrestrial (collection/processing) overprints. The present SXRF microprobe is a simple, yet powerful, instrument in which specimens are excited with filtered, continuum synchrotron radiation from a bending magnet on a 2.5 GeV electron storage ring. A refrigerated cell will be constructed to permit analyses at low temperatures. The cell will consist essentially of an air tight housing with a cold stage. Kapton windows will be used to allow the incident synchrotron beam to enter the cell and fluorescent x rays to exit it. The cell will be either under vacuum or continuous purge by ultrapure helium during analyses. Several other improvements of the NSLS microprobe will be made prior to the cometary nucleus sample return mission that will greatly enhance the sensitivity of the technique.

  16. Graphene oxide windows for in situ environmental cell photoelectron spectroscopy.

    PubMed

    Kolmakov, Andrei; Dikin, Dmitriy A; Cote, Laura J; Huang, Jiaxing; Abyaneh, Majid Kazemian; Amati, Matteo; Gregoratti, Luca; Günther, Sebastian; Kiskinova, Maya

    2011-08-28

    The performance of new materials and devices often depends on processes taking place at the interface between an active solid element and the environment (such as air, water or other fluids). Understanding and controlling such interfacial processes require surface-specific spectroscopic information acquired under real-world operating conditions, which can be challenging because standard approaches such as X-ray photoelectron spectroscopy generally require high-vacuum conditions. The state-of-the-art approach to this problem relies on unique and expensive apparatus including electron analysers coupled with sophisticated differentially pumped lenses. Here, we develop a simple environmental cell with graphene oxide windows that are transparent to low-energy electrons (down to 400 eV), and demonstrate the feasibility of X-ray photoelectron spectroscopy measurements on model samples such as gold nanoparticles and aqueous salt solution placed on the back side of a window. These proof-of-principle results show the potential of using graphene oxide, graphene and other emerging ultrathin membrane windows for the fabrication of low-cost, single-use environmental cells compatible with commercial X-ray and Auger microprobes as well as scanning or transmission electron microscopes.

  17. Fine-scale traverses in cumulate rocks, Stillwater Complex: A lunar analogue study

    NASA Technical Reports Server (NTRS)

    Elthon, Donald

    1988-01-01

    The objective was to document finite-scale compositional variations in cumulate rocks from the Stillwater Complex in Montana and to interpret these data in the context of planetary magma fractionation processes such as those operative during the formation of the Earth's Moon. This research problem involved collecting samples in the Stillwater Complex and analyzing them by electron microprobe, X-ray fluorescence (XRF), and instrumental neutron activation analysis (INAA). The electron microprobe is used to determine the compositions of cumulus and intercumulus phases in the rocks, the XRF is used to determine the bulk-rock major element and trace element (Y, Sr, Rb, Zr, Ni, and Cr) abundances, and the INAA lab. is used to determine the trace element (Sc, Co, Cr, Ni, Ta, Hf, U, Th, and the REE) abundances of mineral separates and bulk rocks.

  18. Asymmetric Distribution of Metals in the Xenopus Laevis Oocyte: a Synchrotron X-Ray Fluorescence Microprobe Study

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

    Popescu, B.F.Gh.; Belak, Z.R.; Ignatyev, K.

    2009-06-04

    The asymmetric distribution of many components of the Xenopus oocyte, including RNA, proteins, and pigment, provides a framework for cellular specialization during development. During maturation, Xenopus oocytes also acquire metals needed for development, but apart from zinc, little is known about their distribution. Synchrotron X-ray fluorescence microprobe was used to map iron, copper, and zinc and the metalloid selenium in a whole oocyte. Iron, zinc, and copper were asymmetrically distributed in the cytoplasm, while selenium and copper were more abundant in the nucleus. A zone of high copper and zinc was seen in the animal pole cytoplasm. Iron was alsomore » concentrated in the animal pole but did not colocalize with zinc, copper, or pigment accumulations. This asymmetry of metal deposition may be important for normal development. Synchrotron X-ray fluorescence microprobe will be a useful tool to examine how metals accumulate and redistribute during fertilization and embryonic development.« less

  19. Asymmetri Distribution of Metals in the Xenopus Laevis Oocyte: a Synchrotron X-Ray Fluorescence Microprobe Study

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

    Popescu, B.F.G.; Belak, Z.R.; Ignatyev, K.

    2009-04-29

    The asymmetric distribution of many components of the Xenopus oocyte, including RNA, proteins, and pigment, provides a framework for cellular specialization during development. During maturation, Xenopus oocytes also acquire metals needed for development, but apart from zinc, little is known about their distribution. Synchrotron X-ray fluorescence microprobe was used to map iron, copper, and zinc and the metalloid selenium in a whole oocyte. Iron, zinc, and copper were asymmetrically distributed in the cytoplasm, while selenium and copper were more abundant in the nucleus. A zone of high copper and zinc was seen in the animal pole cytoplasm. Iron was alsomore » concentrated in the animal pole but did not colocalize with zinc, copper, or pigment accumulations. This asymmetry of metal deposition may be important for normal development. Synchrotron X-ray fluorescence microprobe will be a useful tool to examine how metals accumulate and redistribute during fertilization and embryonic development.« less

  20. Determination of niobium in rocks, ores and alloys by atomic-absorption spectrophotometry.

    PubMed

    Husler, J

    1972-07-01

    Niobium, in concentrations as low as 0.02% Nb(2)O(5), is determined in a variety of materials without separation or enrichment. Chemical and ionization interferences are controlled, and sensitivity is increased, by maintaining the iron, aluminium, hydrofluoric acid and potassium content within certain broad concentration limits. There is close agreement with the results of analyses by emission spectrographic, electron microprobe and X-ray fluorescence methods.

  1. The x ray microprobe determination of chromium oxidation state in olivine from lunar basalt and kimberlitic diamonds

    NASA Technical Reports Server (NTRS)

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

    1993-01-01

    The synchrotron x-ray microprobe is being used to obtain oxidation state information on planetary materials with high spatial resolution. Initial results on chromium in olivine from various sources including laboratory experiments, lunar basalt, and kimberlitic diamonds are reported. The lunar olivine was dominated by Cr(2+) whereas the diamond inclusions had Cr(2+/Cr(3+) ratios up to about 0.3. The simpliest interpretation is that the terrestrial olivine crystallized in a more oxidizing environment than the lunar olivine.

  2. SXRF determination of trace elements in chondrule rims in the unequilibrated CO3 chondrite, ALH A77307

    NASA Technical Reports Server (NTRS)

    Brearley, Adrian J.; Bajt, Sasa; Sutton, Steve R.; Papike, J. J.

    1993-01-01

    The concentrations of Ni, Cu, Zn, Ga, Ge, and Se in five chondrule rims in the CO3 chondrite ALH A77307 (3.0) using the synchrotron x-ray fluorescence (SXRF) microprobe at Brookhaven National Laboratory were determined. The data show that the trace element chemistry of rims on different chondrules is remarkably similar, consistent with data obtained for the major elements by electron microprobe. These results support the idea that rims are not genetically related to individual chondrules, but all sampled the same reservoir of homogeneously mixed dust. Of the trace elements analyzed Zn and Ga show depletions relative to CI chondrite values, but in comparison with bulk CO chondrites all the elements are enriched by approximately 1.5 to 3.5 x CO. The high concentrations of the highly volatile elements Se and Ga and moderately volatile Zn (1.5 to 2 x CO) in rims show that matrix is the major reservoir of volatile elements in ALH A77307.

  3. Laboratory technology and cosmochemistry

    PubMed Central

    Zinner, Ernst K.; Moynier, Frederic; Stroud, Rhonda M.

    2011-01-01

    Recent developments in analytical instrumentation have led to revolutionary discoveries in cosmochemistry. Instrumental advances have been made along two lines: (i) increase in spatial resolution and sensitivity of detection, allowing for the study of increasingly smaller samples, and (ii) increase in the precision of isotopic analysis that allows more precise dating, the study of isotopic heterogeneity in the Solar System, and other studies. A variety of instrumental techniques are discussed, and important examples of discoveries are listed. Instrumental techniques and instruments include the ion microprobe, laser ablation gas MS, Auger EM, resonance ionization MS, accelerator MS, transmission EM, focused ion-beam microscopy, atom probe tomography, X-ray absorption near-edge structure/electron loss near-edge spectroscopy, Raman microprobe, NMR spectroscopy, and inductively coupled plasma MS. PMID:21498689

  4. Sub-Micrometer Scale Minor Element Mapping in Interplanetary Dust Particles: A Test for Stratospheric Contamination

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Keller, L. P.; Sutton, S. R.

    2004-01-01

    Combined X-ray microprobe (XRM), energy dispersive x-ray fluorescence using a Transmission Electron Microscope (TEM), and electron microprobe measurements have determined that the average bulk chemical composition of the interplanetary dust particles (IDPs) collected from the Earth s stratosphere is enriched relative to the CI meteorite composition by a factor of 2 to 4 for carbon and for the moderately volatile elements Na, K, P, Mn, Cu, Zn, Ga, Ge, and Se, and enriched to approximately 30 times CI for Br. However, Jessberger et al., who have reported similar bulk enrichments using Proton Induced X-ray Emission (PIXE), attribute the enrichments to contamination by meteor-derived atmospheric aerosols during the several weeks these IDPs reside in the Earth s atmosphere prior to collection. Using scanning Auger spectroscopy, a very sensitive surface analysis technique, Mackinnon and Mogk have observed S contamination on the surface of IDPs, presumably due to the accretion of sulfate aerosols during stratospheric residence. But the S-rich layer they detected was so thin (approximately 100 angstroms thick) that the total amount of S on the surface was too small to significantly perturb the bulk S-content of a chondritic IDP. Stephan et al. provide support for the contamination hypothesis by reporting the enrichment of Br on the edges of the IDPs using Time-of-Flight Secondary-Ion Mass-Spectrometry (TOFSIMS), but TOF-SIMS is notorious for producing false edge-effects, particularly on irregularly-shaped samples like IDPs. Sutton et al. mapped the spatial distribution of Fe, Ni, Zn, Br, and Sr, at the approximately 2 m scale, in four IDPs using element-specific x-ray fluorescence (XRF) computed microtomography. They found the moderately volatile elements Zn and Br, although spatially inhomogeneous, were not concentrated on the surface of any of the IDPs they examined, suggesting that the Zn and the Br enrichments in the IDPs are not due to contamination during stratospheric residence.

  5. Increasing the Efficiency of Electron Microprobe Measurements of Minor and Trace Elements in Rutile

    NASA Astrophysics Data System (ADS)

    Neill, O. K.; Mattinson, C. G.; Donovan, J.; Hernández Uribe, D.; Sains, A.

    2016-12-01

    Minor and trace element contents of rutile, an accessory mineral found in numerous lithologic settings, has many applications for interpreting earth systems. While these applications vary widely, they share a need for precise and accurate elemental measurements. The electron microprobe can be used to measure rutile compositions, although long X-ray counting times are necessary to achieve acceptable precision. Continuum ("background") intensity can be estimated using the iterative Mean Atomic Number (MAN) method of Donovan and Tingle (1996), obviating the need for direct off-peak background measurements, and reducing counting times by half. For this study, several natural and synthetic rutiles were measured by electron microprobe. Data was collected once but reduced twice, using off-peak and an MAN background corrections, allowing direct comparison of the two methods without influence of other variables (counting time, analyte homogeneity, beam current, calibration standards, etc.). These measurements show that, if a "blank" correction (Donovan et al., 2011, 2016) is used, minor and trace elements of interest can be measured in rutile using the MAN background method in half the time of traditional off-peak measurements, without sacrificing accuracy or precision (Figure 1). This method has already been applied to Zr-in-rutile thermometry of ultra-high pressure metamorphic rocks from the North Qaidam terrane in northwest China. Finally, secondary fluorescence of adjacent phases by continuum X-rays can lead to artificially elevated concentrations. For example, when measuring Zr, care should be taken to avoid analytical spots within 100 microns of zircon or baddeleyite crystals. References: 1) J.J. Donovan and T.N Tingle (1996) J. Microscopy, 2(1), 1-7 2) J.J. Donovan, H.A. Lowers, and B.G. Rusk (2011) Am. Mineral., 96, 274­282 3) J.J. Donovan, J.W. Singer and J.T. Armstrong (2016) Am. Mineral., 101, 1839-1853 4) G.L. Lovizotto et al. (2009) Chem. Geol., 261, 346-369

  6. Oxidation in oxygen at 900 deg and 1000 deg C of four nickel-base cast superalloys: NASA-TRW VIA, B-1900, alloy 713C, and IN-738

    NASA Technical Reports Server (NTRS)

    Fryburg, G. C.; Kohl, F. J.; Stearns, C. A.

    1977-01-01

    The oxidation at 900 and 1,000 C of four nickel-base superalloys in 1 atmosphere of slowly flowing oxygen was investigated. Thermogravimetric rate data were obtained for periods to 100 hours. The morphology and composition of the oxide scales formed after 100 hours were studied by optical microscopy, X-ray diffraction, electron microprobe, scanning electron microscopy, and X-ray photoelectron spectroscopy (ESCA). Alloys B-1900 and VIA were found to be primarily alumina formers, though probably 25 percent of their surface was covered by CR2O3-containing oxides at 900 C. Alloys 713C and IN-738 were primarily chromia formers, though the surface of 713C at 1,000 C was covered with NiO, and the surface of IN-738 at both temperatures was covered with a thin layer of TiO2.

  7. XAFS and X-Ray and Electron Microscopy Investigations of Radionuclide Transformations at the Mineral-Microbe Interface

    NASA Astrophysics Data System (ADS)

    Kemner, Ken; O'Loughlin, Ed; Kelly, Shelly; Ravel, Bruce; Boyanov, Maxim; Sholto-Douglas, Deirdre; Lai, Barry; Cook, Russ; Carpenter, Everett; Harris, Vince; Nealson, Ken

    2007-02-01

    The microenvironment at and adjacent to surfaces of actively metabolizing cells, whether in a planktonic state or adhered to mineral surfaces, can be significantly different from the bulk environment. Microbial polymers (polysaccharides, DNA, RNA, and proteins), whether attached to or released from the cell, can contribute to the development of steep chemical gradients over very short distances. It is currently difficult to predict the behavior of contaminant radionuclides and metals in such microenvironments, because the chemistry there has been difficult or impossible to define. The behavior of contaminants in such microenvironments can ultimately affect their macroscopic fates. We have successfully performed a series of U LIII edge x-ray absorption fine structure (XAFS) spectroscopy, hard x-ray fluorescence (XRF) microprobe (150 nm resolution), and electron microscopy (EM) measurements on lepidocrocite thin films (˜1 micron thickness) deposited on kapton films that have been inoculated with the dissimilatory metal reducing bacterium Shewanella oneidensis MR-1 and exposed to 0.05 mM uranyl acetate under anoxic conditions. Similarly, we have performed a series of U LIII edge EXAFS measurements on lepidocrocite powders exposed to 0.05 mM uranyl acetate and exopolymeric components harvested from S. oneidensis MR-1 grown under aerobic conditions. These results demonstrate the utility of combining bulk XAFS with x-ray and electron microscopies.

  8. Chemical processes involved in the initiation of hot corrosion of B-1900 and NASA-TRW VIA

    NASA Technical Reports Server (NTRS)

    Fryburg, G. C.; Kohl, F. J.; Stearns, C. A.

    1979-01-01

    Sodium sulfate induced hot corrosion of B-1900 and NASA-TRW VIA at 900 C was studied with special emphasis on the chemical reactions occurring during and immediately after the induction period. Thermogravimetric tests were run for set periods of time after which the samples were washed with water and water soluable metal salts and/or residual sulfates were analyzed chemically. Element distributions within the oxide layer were obtained from electron microprobe X-ray micrographs. A third set of samples were subjected to surface analysis by X-ray photoelectron spectroscopy. Evolution of SO2 was monitored throughout many of the hot corrosion tests. Results are interpreted in terms of acid-base fluxing mechanisms.

  9. Mineralogical characterization of rendering mortars from decorative details of a baroque building in Kozuchow (SW Poland)

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

    Bartz, W., E-mail: wojciech.bartz@ing.uni.wroc.pl; Filar, T.

    Optical microscopic observations, scanning electron microscopy and microprobe with energy dispersive X-ray analysis, X-ray diffraction and differential thermal/thermogravimetric analysis allowed detailed characterization of rendering mortars from decorative details (figures of Saints) of a baroque building in Kozuchow (Lubuskie Voivodship, Western Poland). Two separate coats of rendering mortars have been distinguished, differing in composition of their filler. The under coat mortar has filler composed of coarse-grained siliceous sand, whereas the finishing one has much finer grained filler, dominated by a mixture of charcoal and Fe-smelting slag, with minor amounts of quartz grains. Both mortars have air-hardening binder composed of gypsum andmore » micritic calcite, exhibiting microcrystalline structure.« less

  10. Microscopic and Metallurgical Aspects of the Space Shuttle Columbia Accident Investigation and Reconstruction

    NASA Technical Reports Server (NTRS)

    McDaniels, Steven J.

    2004-01-01

    The Space Shuttle Columbia was descending for a landing at the Kennedy Space Center (KSC) on February 1, 2003. Approximately 20 minutes prior to touchdown, the Columbia began disintegrating over the western United States; the majority of debris eventually impacted in eastern Texas and western Louisiana. A monumental effort eventually recovered approximately 84,000 pieces of debris, approximately 38% of the Orbiter's original dry weight. The debris was transported to KSC, where the items were catalogued and evaluated. Critical areas of interest, such as the left and right leading edge surfaces and the underside of the ship, were placed upon a grid to aid in the reconstruction. Items of interest included metallic structures, reinforced carbon-carbon composites, and ceramic heat insulation tiles. Many of the leading edge elements had re-solidified metallic deposits spattered on them. These deposits became known as slag and were one of the main focuses of the investigation. In order to help determine the sequence of events inside the left wing during the accident, the slag's composition, layering order, and directionality of deposition were studied. A myriad of analytical tests were performed in an attempt to ascertain the compositional and depositional characteristics of selected slag deposits, including the ordering of deposited layers within each individual slag deposit harvested. Initially, Scanning Electron Microscopy and Energy Dispersive X-Ray Spectroscopy (SEM/EDX) were performed to quickly characterize the overall composition of individual slag deposits: SEM utilizes a narrowlyfocused high-energy electron beam impinging upon a specimen. The incident beam excites and liberates lower energy secondary electrons, which are detected and analyzed, providing a visual representation of the sample's surface topography. EDX also relies on an incident electron beam, except an EDX unit measures X-ray energies generated by the impinging beam. Each element generates a unique X-ray signature; the EDX detector measures these discreet energies. EDX actually penetrates approximately 2 microns into the bulk of the sample. However, random examination of various portions of slag, coupled with the semiquantitative nature of the SEM/EDX analysis, did not yield convincingly pertinent data. Therefore, X-ray dot mapping was conducted, which provided more understandable data, both in terms of slag layering and composition. An X-ray dot map is generated by performing numerous EDX scans for individual elements, then compiling the scans in a visual representation. Eventually, specimens consisting of not only the slag, but of the adjacent RCC substrate as well were cross-sectioned. X-Ray dot mapping of the materialographicallymounted and -polished cross- sections provided a visual representation of both the layering sequence and compositional characteristics of the slag. Contemporaneously, Electron Spectroscopy for Chemical Analysis/X-Ray Photoelectron Spectroscopy (ESCA/XPS) and powdered X-Ray Diffraction (XRD) were performed to further characterize the deposits and to attempt to identify what, if any, compounds were present. The ESCA/XPS analysis allowed the analyst to "sputter" into the sample with an electron gun, aiding in the identification of the layering sequence. XPS uses photons, rather than electrons, which impinge upon the surface of the sample. XPS measures the electrons emitted from within the first 5 nm of the sample's surface. The XRD measures the scatter angles of incident X-rays; the angle and intensity of scatter depend upon the crystalline structure of the pulverized sample. XRD is considered a qualitative rather than quantitative technique. ESCA/XPS revealed that the final layer to deposit was predominantly carbonaceous. XRD was successful in identifying specific compounds, such as Al 2O3, Al and/or Al3 21SiO47, mullite (3(Al2)O3 -SiO2), and nickel-aluminides. Eventually, Electron MicroProbe Analysis (EMPA) was conducted on the marialographically-prepared cross- sections of selected slag deposits. Microprobe combines SEM and Wavelength Dispersive X-Ray Spectroscopy (WDS), and, like EDX, uses a narrowly-focused high-energy electron beam impinging upon a specimen to elicit, in the case of EPMA, characteristic X-rays with specific wavelengths. This quantitative, analytical tool proved the most useful in determining depositional layering and composition of the slag deposits. This information was utilized in verifying the location of the breach in the left leading edge of the wing of the Columbia.

  11. The solubility and site preference of Fe3+ in Li7−3xFexLa3Zr2O12 garnets

    PubMed Central

    Rettenwander, D.; Geiger, C.A.; Tribus, M.; Tropper, P.; Wagner, R.; Tippelt, G.; Lottermoser, W.; Amthauer, G.

    2015-01-01

    A series of Fe3+-bearing Li7La3Zr2O12 (LLZO) garnets was synthesized using solid-state synthesis methods. The synthetic products were characterized compositionally using electron microprobe analysis and inductively coupled plasma optical emission spectroscopy (ICP-OES) and structurally using X-ray powder diffraction and 57Fe Mössbauer spectroscopy. A maximum of about 0.25 Fe3+ pfu could be incorporated in Li7−3xFexLa3Zr2O12 garnet solid solutions. At Fe3+ concentrations lower than about 0.16 pfu, both tetragonal and cubic garnets were obtained in the synthesis experiments. X-ray powder diffraction analysis showed only a garnet phase for syntheses with starting materials having intended Fe3+ contents lower than 0.52 Fe3+ pfu. Back-scattered electron images made with an electron microprobe also showed no phase other than garnet for these compositions. The lattice parameter, a0, for all solid-solution garnets is similar with a value of a0≈12.98 Å regardless of the amount of Fe3+. 57Fe Mössbauer spectroscopic measurements indicate the presence of poorly- or nano-crystalline FeLaO3 in syntheses with Fe3+ contents greater than 0.16 Fe3+ pfu. The composition of different phase pure Li7−3xFexLa3Zr2O12 garnets, as determined by electron microprobe (Fe, La, Zr) and ICP-OES (Li) measurements, give Li6.89Fe0.03La3.05Zr2.01O12, Li6.66Fe0.06La3.06Zr2.01O12, Li6.54Fe0.12La3.01Zr1.98O12, and Li6.19Fe0.19La3.02Zr2.04O12. The 57Fe Mössbauer spectrum of cubic Li6.54Fe0.12La3.01Zr1.98O12 garnet indicates that most Fe3+ occurs at the special crystallographic 24d position, which is the standard tetrahedrally coordinated site in garnet. Fe3+ in smaller amounts occurs at a general 96h site, which is only present for certain Li-oxide garnets, and in Li6.54Fe0.12La3.01Zr1.98O12 this Fe3+ has a distorted 4-fold coordination. PMID:26435549

  12. Oxidation of silicon nitride sintered with rare-earth oxide additions

    NASA Technical Reports Server (NTRS)

    Mieskowski, D. M.; Sanders, W. A.

    1985-01-01

    The effects of rare-earth oxide additions on the oxidation of sintered Si3N4 were examined. Insignificant oxidation occurred at 700 and 1000 C, with no evidence of phase instability. At 1370 C, the oxidation rate was lowest for Y2O3 and increased for additions of La2O3, Sm2O3, and CeO2, in that order. Data obtained from X-ray diffraction, electron microprobe analysis, and scanning electron microscopy indicate that oxidation occurs via diffusion of cationic species from Si3N4 grain boundaries.

  13. µ-XANES AND µ-XRF INVESTIGATIONS OF METAL BINDING MECHANISMS IN BIOSOLIDS

    EPA Science Inventory

    Micro-X-ray fluorescence (µ-XRF) microprobe analysis and micro-X-ray absorption near edge spectroscopy (µ-XANES) were employed to identify Fe and Mn phases and their association with selected toxic elements in two biosolids (limed composted and Nu-Earth) containing low ...

  14. Aplanatic and quasi-aplanatic diffraction gratings

    DOEpatents

    Hettrick, M.C.

    1987-09-14

    A reflection diffraction grating having a series of transverse minute grooves of progressively varying spacing along a concave surface enables use of such gratings for x-ray or longer wavelength imaging of objects. The variable groove spacing establishes aplanatism or substantially uniform magnetification across the optical aperture. The grating may be sued, for example, in x-ray microscopes or telescopes of the imaging type and in x-ray microprobed. Increased spatial resolution and field of view may be realized in x-ray imaging. 5 figs.

  15. Characterization of crust formation on a parent body of achondrites and the moon by pyroxene crystallography and chemistry

    NASA Technical Reports Server (NTRS)

    Takeda, H.; Miyamoto, M.; Ishii, T.; Reid, A. M.

    1976-01-01

    Single crystal X-ray diffraction and electron microprobe techniques were used to study lunar crustal pyroxenes in a cataclastic norite, a pyroxene-rich clast, and anorthosite lunar samples, and also in meteorites including diogenites, eucrites, and the Yamoto (1) howardite. The crystallographic and chemical characteristics of pyroxenes in these materials are compared and are discussed in terms of the lower stability limit of pigeonite. A mechanical mixing model of howardite is proposed.

  16. Synchrotron X-Ray Microprobe In-Situ Analysis of Extraterrestrial Particles Collected in Aerogel on the MIR Space Station

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Sutton, S. R.; Horz, F.

    2000-01-01

    Using in-situ x-ray fluorescence, we determined the Cr/Fe, Mn/Fe and Ni/Fe of a particle captured in aerogel on MIR are approximately chondritic, indicating an extraterrestrial origin. Impurity of the aerogel precluded determining the Cu and Zn.

  17. The X-ray Fluorescence Microscopy Beamline at the Australian Synchrotron

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

    Paterson, D.; Jonge, M. D. de; Howard, D. L.

    2011-09-09

    A hard x-ray micro-nanoprobe has commenced operation at the Australian Synchrotron providing versatile x-ray fluorescence microscopy across an incident energy range from 4 to 25 keV. Two x-ray probes are used to collect {mu}-XRF and {mu}-XANES for elemental and chemical microanalysis: a Kirkpatrick-Baez mirror microprobe for micron resolution studies and a Fresnel zone plate nanoprobe capable of 60-nm resolution. Some unique aspects of the beamline design and operation are discussed. An advanced energy dispersive x-ray fluorescence detection scheme named Maia has been developed for the beamline, which enables ultrafast x-ray fluorescence microscopy.

  18. Hg diffusion in books of XVIII and XIX centuries by synchrotron microprobe

    NASA Astrophysics Data System (ADS)

    Pessanha, S.; Carvalho, M. L.; Manso, M.; Guilherme, A.; Marques, A. F.; Perez, C. A.

    2009-08-01

    The pigment vermilion (HgS) was used to color the fore edge, tail and head of books. Dissemination and quantification of Hg present in the ink used to color books from XVIII and XIX centuries are reported. Mercury is a very toxic element for the human body, therefore it is extremely important to know whether Hg tends to disseminate throughout the paper or stays confined to the borders of the books with less danger for readers. Synchrotron X-ray microprobe was used to evaluate Hg dissemination from the border to the centre of the paper sheet. The diffusion pattern of Hg was compared with the results obtained by a portable X-ray fluorescence spectrometer and mean quantitative calculations were obtained by a stationary X-ray fluorescence system with triaxial geometry. The results showed high concentrations of Hg in the external regions, but no diffusion was observed for the inner parts of the paper.

  19. Electron microprobe analysis and histochemical examination of the calcium distribution in human bone trabeculae: a methodological study using biopsy specimens from post-traumatic osteopenia

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

    Obrant, K.J.; Odselius, R.

    1984-01-01

    Energy dispersive X-ray microanalysis (EDX) (or electron microprobe analysis) of the relative intensity for calcium in different bone trabeculae from the tibia epiphysis, and in different parts of one and the same trabecula, was performed on 3 patients who had earlier had a fracture of the ipsilateral tibia-diaphysis. The variation in intensity was compared with the histochemical patterns obtained with both the Goldner and the von Kossa staining techniques for detecting calcium in tissues. Previously reported calcium distribution features, found to be typical for posttraumatic osteopenia, such as striated mineralization patterns in individual trabeculae and large differences in mineralization levelmore » between different trabeculae, could be verified both by means of the two histochemical procedures and from the electron microprobe analysis. A pronounced difference was observed, however, between the two histochemical staining techniques as regards their sensitivity to detect calcium. To judge from the values obtained from the EDX measurements, the sensitivity of the Goldner technique should be more than ten times higher than that of von Kossa. The EDX measurements gave more detailed information than either of the two histochemical techniques: great variations in the intensity of the calcium peak were found in trabeculae stained as unmineralized as well as mineralized.« less

  20. Measurement of carbon distribution in nuclear fuel pin cladding specimens by means of a secondary ion mass spectrometer

    NASA Astrophysics Data System (ADS)

    Bart, Gerhard; Aerne, Ernst Tino; Burri, Martin; Zwicky, Hans-Urs

    1986-11-01

    Cladding carburization during irradiation of advanced mixed uranium plutonium carbide fast breeder reactor fuel is possibly a life limiting fuel pin factor. The quantitative assessment of such clad carbon embrittlement is difficult to perform by electron microprobe analysis because of sample surface contamination, and due to the very low energy of the carbon K α X-ray transition. The work presented here describes a method developed at the Swiss Federal Institute for Reactor Research (EIR) to use shielded secondary ion mass spectrometry (SIMS) as an accurate tool to determine radial distribution profiles of carbon in radioactive stainless steel fuel pin cladding. Compared with nuclear microprobe analysis (NMA) [1], which is also an accurate method for carbon analysis, the SIMS method distinguishes itself by its versatility for simultaneous determination of additional impurities.

  1. Layer dependence of the superconducting transition temperature of HgBa2Can-1 CunO2 n+2+ δ

    NASA Astrophysics Data System (ADS)

    Scott, B. A.; Suard, E. Y.; Tsuei, C. C.; Mitzi, D. B.; McGuire, T. R.; Chen, B.-H.; Walker, D.

    1994-09-01

    High-pressure methods have been used to synthesize multiphase compositions in the Hg12{ n-1} n homologous series. The phase assemblages were examined by optical, electron diffraction and X-ray diffraction techniques, and their stoichiometries verified by electron microprobe. Transport and magnetic susceptibility measurements were combined with the results of the phase analysis to establish superconducting transition temperatures for both as-prepared and O 2- or Ar-annealed materials. It was found that the transition temperature peaks at Tc = 134 K for n = 3 and then decreases abruptly for n>4, reaching Tc<90 K for n⪖7.

  2. X-ray microprobe synchroton radiation X-ray fluorescence application on human teeth of renal insufficiency patients

    NASA Astrophysics Data System (ADS)

    Marques, A. F.; Marques, J. P.; Casaca, C.; Carvalho, M. L.

    2004-10-01

    This work reports on the measurements of elemental profiles in teeth collected from patients with renal insufficiency. Elemental concentrations of Ti, Mn, Fe, Co, Ni, Cu, Zn, Se, Br, Rb Sr and Pb in different parts of teeth from patients with renal insufficiency are discussed and correlated with the corresponding values for healthy citizens. Both situations, patients with and without dialysis treatment were studied. The purpose of this work is to point out the influence of renal insufficiency together with long dialysis treatment, on teeth elemental content. An X-ray fluorescence set-up with microprobe capabilities, installed at the LURE synchrotron (France) was used for elemental determination. The resolution of the synchrotron microprobe was 100 μm and the energy of the incident photons was 19 keV. Teeth of citizens with renal insufficiency and those submitted since several years to dialysis treatment show a similar concentration with teeth of healthy subjects in what concerns the elemental distribution for Mn, Fe, Cu, Zn and Sr. However, higher levels of Pb were found in pulp region of diseased citizens when compared to values of healthy people. Very low concentrations of Ti, Co, Ni, Se, Br and Rb were found in all the analysed teeth. No difference was found in patients with and without dialysis treatment.

  3. Simultaneous assessment of phase chemistry, phase abundance and bulk chemistry with statistical electron probe micro-analyses: Application to cement clinkers

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

    Wilson, William; Krakowiak, Konrad J.; Ulm, Franz-Josef, E-mail: ulm@mit.edu

    2014-01-15

    According to recent developments in cement clinker engineering, the optimization of chemical substitutions in the main clinker phases offers a promising approach to improve both reactivity and grindability of clinkers. Thus, monitoring the chemistry of the phases may become part of the quality control at the cement plants, along with the usual measurements of the abundance of the mineralogical phases (quantitative X-ray diffraction) and the bulk chemistry (X-ray fluorescence). This paper presents a new method to assess these three complementary quantities with a single experiment. The method is based on electron microprobe spot analyses, performed over a grid located onmore » a representative surface of the sample and interpreted with advanced statistical tools. This paper describes the method and the experimental program performed on industrial clinkers to establish the accuracy in comparison to conventional methods. -- Highlights: •A new method of clinker characterization •Combination of electron probe technique with cluster analysis •Simultaneous assessment of phase abundance, composition and bulk chemistry •Experimental validation performed on industrial clinkers.« less

  4. PROGRESS ON THE STUDY OF THE URANIUM-ALUMINUM-IRON CONSTITUTION DIAGRAM FOR THE PERIOD SEPTEMBER 1-DECEMBER 31, 1963

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

    Russell, R.B.

    The U--Al--Fe constitution diagram up to about 1000 ppm each of aluminum and iron is sthdied. The techniques used for this study include optical, electron, and x-ray metallography; microprobe analysis, electric conductivity, and hardness measurements. A combination of techniques are giving evidence of the amount of solid solubility of aluminum and iron in alpha, beta, and gamma uranium at selected higher temperatures. The U-Al and U-Fe phase diagrams are also being determined. (N.W.R.)

  5. Correction factors for on-line microprobe analysis of multielement alloy systems

    NASA Technical Reports Server (NTRS)

    Unnam, J.; Tenney, D. R.; Brewer, W. D.

    1977-01-01

    An on-line correction technique was developed for the conversion of electron probe X-ray intensities into concentrations of emitting elements. This technique consisted of off-line calculation and representation of binary interaction data which were read into an on-line minicomputer to calculate variable correction coefficients. These coefficients were used to correct the X-ray data without significantly increasing computer core requirements. The binary interaction data were obtained by running Colby's MAGIC 4 program in the reverse mode. The data for each binary interaction were represented by polynomial coefficients obtained by least-squares fitting a third-order polynomial. Polynomial coefficients were generated for most of the common binary interactions at different accelerating potentials and are included. Results are presented for the analyses of several alloy standards to demonstrate the applicability of this correction procedure.

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

    Reusch, L. M., E-mail: lmmcguire@wisc.edu; Den Hartog, D. J.; Goetz, J.

    The two-color soft x-ray (SXR) tomography diagnostic on the Madison Symmetric Torus is capable of making electron temperature measurements via the double-filter technique; however, there has been a 15% systematic discrepancy between the SXR double-filter (SXR{sub DF}) temperature and Thomson scattering (TS) temperature. Here we discuss calibration of the Be filters used in the SXR{sub DF} measurement using empirical measurements of the transmission function versus energy at the BESSY II electron storage ring, electron microprobe analysis of filter contaminants, and measurement of the effective density. The calibration does not account for the TS and SXR{sub DF} discrepancy, and evidence frommore » experiments indicates that this discrepancy is due to physics missing from the SXR{sub DF} analysis rather than instrumentation effects.« less

  7. The solubility and site preference of Fe{sup 3+} in Li{sub 7−3x}Fe{sub x}La{sub 3}Zr{sub 2}O{sub 12} garnets

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

    Rettenwander, D., E-mail: daniel.rettenwander@sbg.ac.at; Geiger, C.A.; Tribus, M.

    2015-10-15

    A series of Fe{sup 3+}-bearing Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (LLZO) garnets was synthesized using solid-state synthesis methods. The synthetic products were characterized compositionally using electron microprobe analysis and inductively coupled plasma optical emission spectroscopy (ICP-OES) and structurally using X-ray powder diffraction and {sup 57}Fe Mössbauer spectroscopy. A maximum of about 0.25 Fe{sup 3+} pfu could be incorporated in Li{sub 7−3x}Fe{sub x}La{sub 3}Zr{sub 2}O{sub 12} garnet solid solutions. At Fe{sup 3+} concentrations lower than about 0.16 pfu, both tetragonal and cubic garnets were obtained in the synthesis experiments. X-ray powder diffraction analysis showed only a garnet phase for syntheses withmore » starting materials having intended Fe{sup 3+} contents lower than 0.52 Fe{sup 3+} pfu. Back-scattered electron images made with an electron microprobe also showed no phase other than garnet for these compositions. The lattice parameter, a{sub 0}, for all solid-solution garnets is similar with a value of a{sub 0}≈12.98 Å regardless of the amount of Fe{sup 3+}. {sup 57}Fe Mössbauer spectroscopic measurements indicate the presence of poorly- or nano-crystalline FeLaO{sub 3} in syntheses with Fe{sup 3+} contents greater than 0.16 Fe{sup 3+} pfu. The composition of different phase pure Li{sub 7−3x}Fe{sub x}La{sub 3}Zr{sub 2}O{sub 12} garnets, as determined by electron microprobe (Fe, La, Zr) and ICP-OES (Li) measurements, give Li{sub 6.89}Fe{sub 0.03}La{sub 3.05}Zr{sub 2.01}O{sub 12}, Li{sub 6.66}Fe{sub 0.06}La{sub 3.06}Zr{sub 2.01}O{sub 12}, Li{sub 6.54}Fe{sub 0.12}La{sub 3.01}Zr{sub 1.98}O{sub 12}, and Li{sub 6.19}Fe{sub 0.19}La{sub 3.02}Zr{sub 2.04}O{sub 12}. The {sup 57}Fe Mössbauer spectrum of cubic Li{sub 6.54}Fe{sub 0.12}La{sub 3.01}Zr{sub 1.98}O{sub 12} garnet indicates that most Fe{sup 3+} occurs at the special crystallographic 24d position, which is the standard tetrahedrally coordinated site in garnet. Fe{sup 3+} in smaller amounts occurs at a general 96h site, which is only present for certain Li-oxide garnets, and in Li{sub 6.54}Fe{sub 0.12}La{sub 3.01}Zr{sub 1.98}O{sub 12} this Fe{sup 3+} has a distorted 4-fold coordination. - Graphical abstract: Cubic nominally Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (LLZO) garnet is a promising candidate to be used as a solid electrolyte in Li-ion batteries. A series of Fe{sup 3+}-bearing LLZO garnets was synthesized and characterized compositionally and structurally. {sup 57}Mössbauer measurements were made to determine where Fe is incorporated in the crystal structure. X-ray diffraction, electron microprobe, ICP-OES and {sup 57}Mössbauer measurements are needed to obtain a full description of the synthetic products, some of which contain small amounts of nano- or poorly crystalline FeLaO{sub 3}. - Highlights: • A series of Fe{sup 3+}-bearing Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (LLZO) garnets was synthesized and characterized compositionally and structurally. • {sup 57}Mössbauer measurements were made to determine where Fe is incorporated in the crystal structure. • Most Fe{sup 3+} substitutes for Li{sup +} in LLZO at the 24d and 96h sites in the cubic phase (Ia-3d). • No more than about 0.25 Fe{sup 3+} pfu can be incorporated into the LLZO garnet structure. • X-ray powder diffractions measurements indicate the presence of both cubic and tetragonal garnets phases in some syntheses. • The probable presence of small amounts of poorly or nano-crystalline FeLaO3 can only be identified by Mössbauer spectroscopy.« less

  8. Use of electron microprobe x-ray analysis for determination of low calcium concentrations across leaves deficient in calcium

    NASA Technical Reports Server (NTRS)

    Barta, D. J.; Tibbitts, T. W.

    1991-01-01

    An electron microprobe with wavelength-dispersive x-ray spectrometry (WDS) was found to be useful for the determination of Ca concentrations in leaf tissue deficient in Ca. WDS effectively detected Ca concentrations as low as 0.2 mg/g dry wt in the presence of high levels of K and Mg (120 and 50 mg/g dry wt, respectively). Leaf specimens were prepared for analysis by quick-freezing in liquid nitrogen and freeze-drying at -20 degrees C to maintain elemental integrity within the tissue. Because dry material was analyzed, sample preparation was simple and samples could be stored for long periods before analysis. A large beam diameter of 50 gm was used to minimize tissue damage under the beam and analyze mineral concentrations within several cells at one time. Beam penetration was between 50 and 55 microns, approximately one-third of the thickness of the leaf. For analysis of concentrations in interveinal areas, analyses directed into the abaxial epidermis were found most useful. However, because of limited beam penetration, analyses of veinal areas would require use of cross sections [correction of crosssections]. Solid mineral standards were used for instrument standardization. To prevent measurement errors resulting from differences between the matrix of the mineral standards and the analyzed tissue, concentrations in leaves were corrected using gelatin standards prepared and analyzed under the same conditions. WDS was found to be useful for documenting that very low Ca levels occur in specific areas of lettuce leaves exhibiting the Ca deficiency injury termed tipburn.

  9. Soft X-ray and cathodoluminescence measurement, optimisation and analysis at liquid nitrogen temperatures

    NASA Astrophysics Data System (ADS)

    MacRae, C. M.; Wilson, N. C.; Torpy, A.; Delle Piane, C.

    2018-01-01

    Advances in field emission gun electron microprobes have led to significant gains in the beam power density and when analysis at high resolution is required then low voltages are often selected. The resulting beam power can lead to damage and this can be minimised by cooling the sample down to cryogenic temperatures allowing sub-micrometre imaging using a variety of spectrometers. Recent advances in soft X-ray emission spectrometers (SXES) offer a spectral tool to measure both chemistry and bonding and when combined with spectral cathodoluminescence the complementary techniques enable new knowledge to be gained from both mineral and materials. Magnesium and aluminium metals have been examined at both room and liquid nitrogen temperatures by SXES and the L-emission Fermi-edge has been observed to sharpen at the lower temperatures directly confirming thermal broadening of the X-ray spectra. Gains in emission intensity and resolution have been observed in cathodoluminescence for liquid nitrogen cooled quartz grains compared to ambient temperature quartz. This has enabled subtle growth features at quartz to quartz-cement boundaries to be imaged for the first time.

  10. Les fards rouges cosmétiques et rituels a base de cinabre et d'ocre de l'époque punique en Tunisie: analyse, identification et caractérisation.

    PubMed

    Alatrache, A; Mahjoub, H; Ayed, N; Ben Younes, H

    2001-10-01

    Natural antique colorants include mainly red pigments such as cinnabar and ochre. These archeological pigments were used especially as funeral and cosmetic makeup and are a material proof of handicraft activities and exchanges. The identification and characterization of a group of punic colorants, corresponding to samples discovered during excavations at several Tunisian archeological sites (Cartage, Ksour Essef, Kerkouane, Bekalta, Makthar, Bou Arada), were conducted using the least destructive analysis techniques such us scanning electron microscopy coupled to X-ray fluorescence microprobe, direct current plasma emission spectroscopy, atomic absorption spectrometry, Fourier transform infrared spectrometry and X-ray diffraction. Eleven natural red colorants from punic period were subject to this investigation and were compared to contemporary substances. Five colorants were cinnabar and the other six were ochre.

  11. Ted Hall and the science of biological microprobe X-ray analysis: a historical perspective of methodology and biological dividends.

    PubMed

    Gupta, B L

    1991-06-01

    This review surveys the emergence of electron probe X-ray microanalysis as a quantitative method for measuring the chemical elements in situ. The extension of the method to the biological sciences under the influence of Ted Hall is reviewed. Some classical experiments by Hall and his colleagues in Cambridge, UK, previously unpublished, are described; as are some of the earliest quantitative results from the cryo-sections obtained in Cambridge and elsewhere. The progress of the methodology is critically evaluated from the earliest starts to the present state of the art. Particular attention has been focused on the application of the method in providing fresh insights into the role of ions in cell and tissue physiology and pathology. A comprehensive list of references is included for a further pursuit of the topics by the interested reader.

  12. Chemical fingerprinting and source tracing of obsidian: the central Mediterranean trade in black gold.

    PubMed

    Tykot, Robert H

    2002-08-01

    Chemical fingerprinting using major or trace element composition is used to characterize the Mediterranean island sources of obsidian and can even differentiate as many as nine flows in the Monte Arci region of Sardinia. Analysis of significant numbers of obsidian artifacts from Neolithic sites in the central Mediterranean reveals specific patterns of source exploitation and suggests particular trade mechanisms and routes. The use of techniques such as X-ray fluorescence, the electron microprobe, neutron activation analysis, and laser ablation ICP mass spectrometry are emphasized in order to produce quantitative results while minimizing damage to valuable artifacts.

  13. Annealing effects in plated-wire memory elements. I - Interdiffusion of copper and Permalloy.

    NASA Technical Reports Server (NTRS)

    Knudson, C. I.; Kench, J. R.

    1971-01-01

    Results of investigations using X-ray diffraction and electron-beam microprobe techniques have shown that copper and Permalloy platings interdiffuse at low temperatures when plated-wire memory elements are annealed for times as short as 50 hr. Measurable interdiffusion between Permalloy platings and gold substrates does not occur in similar conditions. Both magnetic and compositional changes during aging are found to occur by a thermally activated process with activation energies around 38 kcal/mol. It is shown, however, that copper-diffusion and magnetic-dispersion changes during aging are merely concurrent processes, neither being the other's cause.

  14. Scanning proton microprobe applied to analysis of individual aerosol particles from Amazon Basin

    NASA Astrophysics Data System (ADS)

    Gerab, Fábio; Artaxo, Paulo; Swietlicki, Erik; Pallon, Jan

    1998-03-01

    The development of the Scanning Proton Microprobe (SPM) offers a new possibility for individual aerosol particle studies. The SPM joins Particle Induced X-ray Emission (PIXE) elemental analysis qualities with micrometric spatial resolution. In this work the Lund University SPM facility was used for elemental characterization of individual aerosol particles emitted to the atmosphere in the Brazilian Amazon Basin, during gold mining activities by the so-called "gold shops".

  15. X-ray Mapping of Terrestrial and Extraterrestrial Materials Using the Electron Microprobe

    NASA Technical Reports Server (NTRS)

    Carpenter, P.

    2006-01-01

    Lunar samples returned from the Apollo program motivated development of the Bence-Albee algorithm for the rapid and accurate analysis of lunar materials, and established interlaboratory comparability through its common use. In the analysis of mineral and rock fragments it became necessary to combine micro- and macroscopic analysis by coupling electron-probe microanalysis (EPMA) with automated stage point counting. A coarse grid that included several thousand points was used, and initially wavelength-dispersive (WDS) and later energydispersive (EDS) data were acquired at discrete stage points using approx. 5 sec count times. A approx 50 micrometer beam diameter was used for WDS and up to 500 micrometer beam diameter for EDS analysis. Average analyses of discretely sampled phases were coupled with the point count data to calculate the bulk composition using matrix algebra. Use of a defocused beam resulted in a contribution from multiple phases to each analytical point, and the analytical data were deconvolved relative to end-member phase chemistry on the fly. Impressive agreement was obtained between WDS and EDS measurements as well as comparison with bulk chemistry obtained by other methods. In the 30 years since these methods were developed, significant improvements in EPMA automation and computer processing have taken place. Digital beam control allows routine collection of x-ray maps by EDS, and stage mapping for WDS is conducted continuously at slew speed and incrementally by sampling at discrete points. Digital pulse processing in EDS systems has significantly increased the throughput for EDS mapping, and the ongoing development of Si-drift detector systems promises mapping capabilities rivaling WDS systems. Spectrum imaging allows a data cube of EDS spectra to be acquired and sophisticated processing of the original data is possible using matrix algebra techniques. The study of lunar and meteoritic materials includes the need to conveniently: (1) Characterize the sample at microscopic and macroscopic scales with relatively high sensitivity, (2) Determine the modal abundance of minerals, and (3) Identify and relocate discrete features of interest in terms of size and chemistry. The coupled substitution of cations in minerals can result in significant variation in mineral chemistry, but at similar average Z, leading to poor backscattered-electron (BSE) contrast discrimination of mineralogy. It is necessary to discriminate phase chemistry at both the trace element level and the major element level. To date, the WDS of microprobe systems is preferred for mapping due to high throughput and the ability to obtain the necessary intensity to discriminate phases at both trace and major element concentrations. It is desirable to produce fully quantitative compositional maps of geological materials, which requires the acquisition of k-ratio maps that are background and dead-time corrected, and which have been corrected by phi(delta z> or an equivalent algorithm at each pixel. To date, turnkey systems do not allow the acquisition of k-ratio maps and the rigorous correction in this manner. X-ray maps of a chondrule from the Ourique meteorite, and a comb-layered xenolith from the San Francisco volcanic field, have been analyzed and processed to extract phase information. The Ourique meteorite presents a challenge due to relatively low BSE contrast, and has been studied using spectrum imaging. X-ray maps for Si, Mg, and FeK(alpha) were used to produce RGB images. The xenolith sample contains sector-zoned augite, olivine, plagioclase, and basaltic glass. X-ray maps were processed using Lispix and ImageJ software to produce mineral phase maps. The x-ray maps for Mg, Ca, and Ti were used with traceback to generate binary images that were converted to RGB images. These approaches are successful in discriminating phases, but it is desirable to achieve the methods that were used on lunar samples 30 years ago on current microprobe systems. Curnt research includes x-ray mapping analysis of the Dalgety Downs chondrite by micro x-ray fluorescence and spectrum imaging, in collaboration with Kenny Witherspoon of IXRF Systems and Dale Newbury of NIST.

  16. Phase state of a Bi-43 wt % Sn superplastic alloy and its changes under the effect of external mechanical stresses and aging

    NASA Astrophysics Data System (ADS)

    Korshak, V. F.; Chushkina, R. A.; Shapovalov, Yu. A.; Mateichenko, P. V.

    2011-07-01

    Samples of a Bi-43 wt % Sn superplastic alloy have been studied by X-ray diffraction in the ascast state, after compression of as-cast samples to ˜70% on a hydraulic press, after aging in the as-cast and preliminarily compressed state, and using samples deformed under superplastic conditions. The X-ray diffraction studies have been carried out using a DRON-2.0 diffractometer in Cu Kα radiation. The samples aged and deformed under superplasticity conditions have been studied using electron-microprobe analysis in a JSM-820 scanning electron microscope equipped with a LINK AN/85S EDX system. It has been found that the initial structural-phase state of the alloy was amorphous-crystalline. Causes that lead to a change in this state upon deformation and aging are discussed. A conclusion is made that the superplasticity effect manifests itself against the background of processes that are stipulated by the tendency of the initially metastable alloy to phase equilibrium similarly to what is observed in the Sn-38 wt % Pb eutectic alloy studied earlier.

  17. Oxidation characteristics of Ti-25Al-10Nb-3V-1Mo intermetallic alloy

    NASA Technical Reports Server (NTRS)

    Wallace, Terryl A.; Clark, Ronald K.; Sankaran, Sankara N.; Wiedemann, Karl E.

    1990-01-01

    Static oxidation kinetics of the super-alpha 2 titanium-aluminide alloy Ti-25Al-10Nb-3V-1Mo (at. percent) were investigated in air over the temperature range of 650 to 1000 C using thermogravimetric analysis. The oxidation kinetics were complex at all exposure temperatures and displayed up to three distinct oxidation rates. Breakaway oxidation occurred after long exposure times at high temperatures. Oxidation products were determined using x ray diffraction techniques, electron microprobe analysis, and energy dispersive x ray analysis. Oxide scale morphology was examined by scanning electron microscopy of the surfaces and cross sections of oxidized specimens. The oxides during the parabolic stages were compact and multilayered, consisting primarily of TiO2 doped with Nb, a top layer of Al2O3, and a thin bottom layer of TiN. The transition between the second and third parabolic stage was found to be linked to the formation of a TiAl layer at the oxide-metal interface. Porosity was formed during the third stage, causing degradation of the oxide and the beginning of breakaway oxidation.

  18. Microbiologically influenced corrosion: looking to the future.

    PubMed

    Videla, Héctor A; Herrera, Liz K

    2005-09-01

    This review discusses the state-of-the-art of research into biocorrosion and the biofouling of metals and alloys of industrial usage. The key concepts needed to understand the main effects of microorganisms on metal decay, and current trends in monitoring and control strategies to mitigate the deleterious effects of biocorrosion and biofouling are also described. Several relevant cases of biocorrosion studied by our research group are provided as examples: (i) biocorrosion of aluminum and its alloys by fungal contaminants of jet fuels; (ii) sulfate-reducing bacteria (SRB)-induced corrosion of steel; (iii) biocorrosion and biofouling interactions in the marine environment; (iv) monitoring strategies for assessing biocorrosion in industrial water systems; (v) microbial inhibition of corrosion; (vi) use and limitations of electrochemical techniques for evaluating biocorrosion effects. Future prospects in the field are described with respect to the potential of innovative techniques in microscopy (environmental scanning electron microscopy, confocal scanning laser microscopy, atomic force microscopy), new spectroscopic techniques for the study of corrosion products and biofilms (energy dispersion X-ray analysis, X-ray photoelectron spectroscopy, electron microprobe analysis) and electrochemistry (electrochemical impedance spectroscopy, electrochemical noise analysis).

  19. Geochemical and mineralogical controls on metal(loid) mobility in the oxide zone of the Prairie Creek Deposit, NWT

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

    Stavinga, Drew; Jamieson, Heather; Layton-Matthews, Daniel

    2017-02-01

    Prairie Creek is an unmined high grade Zn-Pb-Ag deposit in the southern Mackenzie Mountains of the Northwest Territories, located in a 320 km2 enclave surrounded by the Nahanni National Park reserve. The upper portion of the quartz-carbonate-sulphide vein mineralization has undergone extensive oxidation, forming high grade zones, rich in smithsonite (ZnCO3) and cerussite (PbCO3). This weathered zone represents a significant resource and a potential component of mine waste material. This study is focused on characterizing the geochemical and mineralogical controls on metal(loid) mobility under mine waste conditions, with particular attention to the metal carbonates as a potential source of tracemore » elements to the environment. Analyses were conducted using a combination of microanalytical techniques (electron microprobe, scanning electron microscopy with automated mineralogy, laser-ablation inductively-coupled mass spectrometry, and synchrotron-based element mapping, micro-X-ray diffraction and micro-X-ray absorbance). The elements of interest included Zn, Pb, Ag, As, Cd, Cu, Hg, Sb and Se.« less

  20. Study on Iron Distribution and Electrical Activities at Grain Boundaries in Polycrystalline Silicon Substrate for Solar Cells

    NASA Astrophysics Data System (ADS)

    Arafune, Koji; Ohishi, Eichiro; Sai, Hitoshi; Terada, Yasuko; Ohshita, Yoshio; Yamaguchi, Masafumi

    2006-08-01

    To clarify the role of grain boundaries in iron sinks and carrier recombination centers, iron distributions and their chemical states were studied before and after gettering. They were measured by the X-ray microprobe fluorescence and the X-ray absorption in the near-edge structure using the beamline 37XU at the SPring-8 third-generation synchrotron facility. To determine the crystallographic orientation of the grain boundaries, electron backscatter diffraction measurements were performed. The distribution of electric active defects was characterized by electron-beam-induced current measurements. Before gettering, the iron was distributed in the small grain and its chemical state was similar to that of iron oxide. After gettering, the iron was redistributed along the small angle grain boundary, and its chemical state was similar to the iron silicide complexed with the iron oxide. Regarding the electrical activity, high carrier recombination was observed along the small-angle grain boundary. On the contrary, Σ 3 grain boundaries were relatively weak impurity sinks and showed low recombination activity.

  1. Calibration Issues and Operating System Requirements for Electron-Probe Microanalysis

    NASA Technical Reports Server (NTRS)

    Carpenter, P.

    2006-01-01

    Instrument purchase requirements and dialogue with manufacturers have established hardware parameters for alignment, stability, and reproducibility, which have helped improve the precision and accuracy of electron microprobe analysis (EPMA). The development of correction algorithms and the accurate solution to quantitative analysis problems requires the minimization of systematic errors and relies on internally consistent data sets. Improved hardware and computer systems have resulted in better automation of vacuum systems, stage and wavelength-dispersive spectrometer (WDS) mechanisms, and x-ray detector systems which have improved instrument stability and precision. Improved software now allows extended automated runs involving diverse setups and better integrates digital imaging and quantitative analysis. However, instrumental performance is not regularly maintained, as WDS are aligned and calibrated during installation but few laboratories appear to check and maintain this calibration. In particular, detector deadtime (DT) data is typically assumed rather than measured, due primarily to the difficulty and inconvenience of the measurement process. This is a source of fundamental systematic error in many microprobe laboratories and is unknown to the analyst, as the magnitude of DT correction is not listed in output by microprobe operating systems. The analyst must remain vigilant to deviations in instrumental alignment and calibration, and microprobe system software must conveniently verify the necessary parameters. Microanalysis of mission critical materials requires an ongoing demonstration of instrumental calibration. Possible approaches to improvements in instrument calibration, quality control, and accuracy will be discussed. Development of a set of core requirements based on discussions with users, researchers, and manufacturers can yield documents that improve and unify the methods by which instruments can be calibrated. These results can be used to continue improvements of EPMA.

  2. Development of an external beam nuclear microprobe on the Aglae facility of the Louvre museum

    NASA Astrophysics Data System (ADS)

    Calligaro, T.; Dran, J.-C.; Ioannidou, E.; Moignard, B.; Pichon, L.; Salomon, J.

    2000-03-01

    The external beam line of our facility has been recently equipped with the focusing system previously mounted on a classical nuclear microprobe. When using a 0.1 μm thick Si 3N 4 foil for the exit window and flowing helium on the sample under analysis, a beam spot as small as 10 μm is attainable at a distance of 3 mm from the window. Elemental micromapping is performed by mechanical scanning. An electronic device has been designed which allows XY scanning by moving the sample under the beam by steps down to 0.1 μm. Beam monitoring is carried out by means of the weak X-ray signal emitted by the exit foil and detected by a specially designed Si(Li) detector cooled by Peltier effect. The characteristics of external beams of protons and alpha particles are evaluated by means of resonance scanning and elemental mapping of a grid. An example of application is presented, dealing with elemental micro-mapping of inclusions in gemstones.

  3. Microscale reconstruction of biogeochemical substrates using multimode X-ray tomography and scanning electron microscopy

    NASA Astrophysics Data System (ADS)

    Miller, M.; Miller, E.; Liu, J.; Lund, R. M.; McKinley, J. P.

    2012-12-01

    X-ray computed tomography (CT), scanning electron microscopy (SEM), electron microprobe analysis (EMP), and computational image analysis are mature technologies used in many disciplines. Cross-discipline combination of these imaging and image-analysis technologies is the focus of this research, which uses laboratory and light-source resources in an iterative approach. The objective is to produce images across length scales, taking advantage of instrumentation that is optimized for each scale, and to unify them into a single compositional reconstruction. Initially, CT images will be collected using both x-ray absorption and differential phase contrast modes. The imaged sample will then be physically sectioned and the exposed surfaces imaged and characterized via SEM/EMP. The voxel slice corresponding to the physical sample surface will be isolated computationally, and the volumetric data will be combined with two-dimensional SEM images along CT image planes. This registration step will take advantage of the similarity between the X-ray absorption (CT) and backscattered electron (SEM) coefficients (both proportional to average atomic number in the interrogated volume) as well as the images' mutual information. Elemental and solid-phase distributions on the exposed surfaces, co-registered with SEM images, will be mapped using EMP. The solid-phase distribution will be propagated into three-dimensional space using computational methods relying on the estimation of compositional distributions derived from the CT data. If necessary, solid-phase and pore-space boundaries will be resolved using X-ray differential phase contrast tomography, x-ray fluorescence tomography, and absorption-edge microtomography at a light-source facility. Computational methods will be developed to register and model images collected over varying scales and data types. Image resolution, physically and dynamically, is qualitatively different for the electron microscopy and CT methodologies. Routine CT images are resolved at 10-20 μm, while SEM images are resolved at 10-20 nm; grayscale values vary according to collection time and instrument sensitivity; and compositional sensitivities via EMP vary in interrogation volume and scale. We have so far successfully registered SEM imagery within a multimode tomographic volume and have used standard methods to isolate pore space within the volume. We are developing a three-dimensional solid-phase identification and registration method that is constrained by bulk-sample X-ray diffraction Rietveld refinements. The results of this project will prove useful in fields that require the fine-scale definition of solid-phase distributions and relationships, and could replace more inefficient methods for making these estimations.

  4. X-ray microprobe analysis of platelets. Principles, methods and review of the literature.

    PubMed

    Yarom, R

    1983-01-01

    Platelets are well suited to X-ray microanalysis as there is no need for chemical fixation or sectioning, and the concentrations of calcium and phosphorus are above 10(-3). The principles of the technique, the methods of specimen preparation, instrumental conditions during analysis and ways of quantitation are described. This is followed by a review of published reports and a brief summary of the author's own work in the field.

  5. Optimisation d'analyses de grenat almandin realisees au microscope electronique a balayage

    NASA Astrophysics Data System (ADS)

    Larose, Miguel

    The electron microprobe (EMP) is considered as the golden standard for the collection of precise and representative chemical composition of minerals in rocks, but data of similar quality should be obtainable with a scanning electron microscope (SEM). This thesis presents an analytical protocol aimed at optimizing operational parameters of an SEM paired with an EDS Si(Li) X-ray detector (JEOL JSM-840A) for the imaging, quantitative chemical analysis and compositional X-ray maps of almandine garnet found in pelitic schists from the Canadian Cordillera. Results are then compared to those obtained for the same samples on a JEOL JXA 8900 EMP. For imaging purposes, the secondary electrons and backscattered electrons signals have been used to obtain topographic and chemical contrast of the samples, respectively. The SEM allows the acquisition of images with higher resolution than the EMP when working at high magnifications. However, for millimetric size minerals requiring very low magnifications, the EMP can usually match the imaging capabilities of an SEM. When optimizing images for both signals, the optimal operational parameters to show similar contrasts are not restricted to a unique combination of values. Optimization of operational parameters for quantitative chemical analysis resulted in analytical data with a similar precision and showing good correlation to that obtained with an EMP. Optimization of operational parameters for compositional X-ray maps aimed at maximizing the collected intensity within a pixel as well as complying with the spatial resolution criterion in order to obtain a qualitative compositional map representative of the chemical variation within the grain. Even though various corrections were needed, such as the shadow effect and the background noise removal, as well as the impossibility to meet the spatial resolution criterion because of the limited pixel density available on the SEM, the compositional X-ray maps show a good correlation with those obtained with the EMP, even for concentrations as low as 0,5%. When paired with a rigorous analytical protocol, the use of an SEM equipped with an EDS Si (Li) X-ray detector allows the collection of qualitative and quantitative results similar to those obtained with an EMP for all three of the applications considered.

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

    Macente, A.; Fusseis, F.; Menegon, L.

    Reaction and deformation microfabrics provide key information to understand the thermodynamic and kinetic controls of tectono-metamorphic processes, however they are usually analysed in two dimensions, omitting important information regarding the third spatial dimension. We applied synchrotron-based X-ray microtomography to document the evolution of a pristine olivine gabbro into a deformed omphacite-garnet eclogite in four dimensions, where the 4th dimension is represented by the degree of strain. In the investigated samples, which cover a strain gradient into a shear zone from the Western Gneiss Region (Norway), we focused on the spatial transformation of garnet coronas into elongated clusters of garnets withmore » increasing strain. Our microtomographic data allowed quantification of garnet volume, shape and spatial arrangement evolution with increasing strain. We combined microtomographic observations with light microscope- and backscatter electron images as well as electron microprobe- (EMPA) and electron backscatter diffraction (EBSD) analysis to correlate mineral composition and orientation data with the X-ray absorption signal of the same mineral grains. With increasing deformation, the garnet volume almost triples. In the low strain domain, garnets form a well interconnected large garnet aggregate that develops throughout the entire Page 1 of 52 sample. We also observed that garnet coronas in the gabbros never completely encapsulate olivine grains. In the most highly deformed eclogites, the oblate shapes of garnet clusters reflect a deformational origin of the microfabrics. We interpret the aligned garnet aggregates to direct synkinematic fluid flow and consequently influence the transport of dissolved chemical components. EBSD analyses reveal that garnet show a near-random crystal preferred orientation that testifies no evidence for crystal plasticity. There is, however evidence for minor fracturing, neo-nucleation and overgrowth. Microprobe chemical analysis revealed that garnet compositions progressively equilibrate to eclogite facies, becoming more almandine-rich. We interpret these observations as pointing to a mechanical disintegration of the garnet coronas during strain localisation, and their rearrangement into individual garnet clusters through a combination of garnet coalescence and overgrowth while the rock was deforming.« less

  7. Mach 1 oxidation of thoriated nickel chromium at 1204 C (2200 F)

    NASA Technical Reports Server (NTRS)

    Lowell, C. E.; Sanders, W. A.

    1971-01-01

    TD NiCr was exposed to a Mach 1, 1-atmosphere gas stream at 1204 C for times up to 50 hours. Weight change, metal thickness loss, X-ray diffraction, metallographic, and electron microprobe analyses were made. Neither surface preparation nor thermal cycling had an appreciable effect on the results. Initially, Cr2O3 formed and volatilized, allowing a rapid metal loss rate of 40 microns per hour. After about 1 hour the Cr2O3 broke down, resulting in an NiO overgrowth. The metal loss rate then slowed to 2.5 microns per hour and remained constant to 50 hours.

  8. Phase relations in the system CuMoS

    USGS Publications Warehouse

    Dawei, H.; Chang, L.L.Y.; Knowles, C.R.

    1990-01-01

    Phase relations in the system CuMoS were studied in the temperature range 500-1000 ??C by using the conventional sealed, evacuated glass capsule technique. Reflected-light microscopy, X-ray powder diffraction and electron microprobe analysis were used for phase characterization. The chevrel-type phase, CuxMo3S4, is stable above 600??C, and forms equilibrium assemblages with the cubic Cu2S solid solution, copper, molybdenum, Mo2S3 and MoS2. Its solid solution ranges from Cu1.50-2.00Mo3S4 at 700??C to Cu1.22-2.00Mo3S4 at 1000 ??C. ?? 1990.

  9. STUDY OF URANIUM-ALUMINUM-IRON TERNARY CONSTITUTION DIAGRAM. Progress Report for the Period Ending March 31, 1963

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

    Russell, R.B.

    The determination of the U--Al-- Fe constitution diagram up to about 1000 ppm each of aluminum and iron is now being implemented by a determination of the U--Al and U-- Fe binary systems. The techniques to be used for this study include optical, electron and x-ray metallography, microprobe analysis, electrical resistance, and hothardness measurements. It is expected that a combination of techniques will give evidence of the amount of solid solubility of aluminum and iron in alpha uranium from 300 to 660 deg C, and in beta uranium at selected higher temperatures. (N.W.R.)

  10. Deciphering the Complex Chemistry of Deep-Ocean Particles Using Complementary Synchrotron X-ray Microscope and Microprobe Instruments.

    PubMed

    Toner, Brandy M; German, Christopher R; Dick, Gregory J; Breier, John A

    2016-01-19

    The reactivity and mobility of natural particles in aquatic systems have wide ranging implications for the functioning of Earth surface systems. Particles in the ocean are biologically and chemically reactive, mobile, and complex in composition. The chemical composition of marine particles is thought to be central to understanding processes that convert globally relevant elements, such as C and Fe, among forms with varying bioavailability and mobility in the ocean. The analytical tools needed to measure the complex chemistry of natural particles are the subject of this Account. We describe how a suite of complementary synchrotron radiation instruments with nano- and micrometer focusing, and X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) capabilities are changing our understanding of deep-ocean chemistry and life. Submarine venting along mid-ocean ridges creates hydrothermal plumes where dynamic particle-forming reactions occur as vent fluids mix with deep-ocean waters. Whether plumes are net sources or sinks of elements in ocean budgets depends in large part on particle formation, reactivity, and transport properties. Hydrothermal plume particles have been shown to host microbial communities and exhibit complex size distributions, aggregation behavior, and composition. X-ray microscope and microprobe instruments can address particle size and aggregation, but their true strength is in measuring chemical composition. Plume particles comprise a stunning array of inorganic and organic phases, from single-crystal sulfides to poorly ordered nanophases and polymeric organic matrices to microbial cells. X-ray microscopes and X-ray microprobes with elemental imaging, XAS, and XRD capabilities are ideal for investigating these complex materials because they can (1) measure the chemistry of organic and inorganic constituents in complex matrices, usually within the same particle or aggregate, (2) provide strong signal-to-noise data with exceedingly small amounts of material, (3) simplify the chemical complexity of particles or sets of particles with a focused-beam, providing spatial resolution over 6 orders of magnitude (nanometer to millimeter), (4) provide elemental specificity for elements in the soft-, tender-, and hard-X-ray energies, (5) switch rapidly among elements of interest, and (6) function in the presence of water and gases. Synchrotron derived data sets are discussed in the context of important advances in deep-ocean technology, sample handling and preservation, molecular microbiology, and coupled physical-chemical-biological modeling. Particle chemistry, size, and morphology are all important in determining whether particles are reactive with dissolved constituents, provide substrates for microbial respiration and growth, and are delivered to marine sediments or dispersed by deep-ocean currents.

  11. A new life for the wavelength-dispersive X-ray spectrometer (WDS): incorporation of a silicon drift detector into the WDS for improved quantification and X-ray mapping

    NASA Astrophysics Data System (ADS)

    Wuhrer, R.; Moran, K.

    2018-01-01

    The wavelength-dispersive X-ray spectrometer (WDS) has been around for a long time and the design has not changed much since its original development. The electron microprobe operator using WDS has to be meticulous in monitoring items such as gas flow, gas purity, gas pressure, noise levels of baseline and window, gas flow proportional counter (GFPC) voltage levels, count rate suppression, anode wire contamination and other detector parameters. Recent development and improvements of silicon drift detectors (SDD’s) has allowed the incorporation of a SDD as the X-ray detector in place of the proportional counter (PC) and/or gas flow proportional counter (GFPC). This allows minimal mechanical alteration and no loss of movement range. The superiority of a WDS with a SDD, referred to as SD-WDS, is easily seen once in operation. The SD-WDS removes many artefacts including the worse of all high order diffraction, thus allowing more accurate analysis. The incorporation of the SDD has been found to improve the light and mid element range and consequently improving the detection limit for these elements. It is also possible to obtain much more reliable results at high count rates with almost no change in resolution, gain and zero-peak characteristics of the energy spectrum.

  12. Electrodeposition of actinide compounds from an aqueous ammonium acetate matrix. Experimental development and optimization

    DOE PAGES

    Boll, Rose Ann; Matos, Milan; Torrico, Matthew N.

    2015-03-27

    Electrodeposition is a technique that is routinely employed in nuclear research for the preparation of thin solid films of actinide materials which can be used in accelerator beam bombardments, irradiation studies, or as radioactive sources. The present study investigates the deposition of both lanthanides and actinides from an aqueous ammonium acetate electrolyte matrix. Electrodepositions were performed primarily on stainless steel disks; with yield analysis evaluated using -spectroscopy. Experimental parameters were studied and modified in order to optimize the uniformity and adherence of the deposition while maximizing the yield. The initial development utilized samarium as the plating material, with and withoutmore » a radioactive tracer. As a result, surface characterization studies were performed by scanning electron microscopy, electron microprobe analysis, radiographic imaging, and x-ray diffraction.« less

  13. Determine the yield of micronucleated cells in primary human fibroblasts exposed to focused soft X-rays.

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

    Kevin M. Prise

    This project was a small part of a larger collaborative study headed by Dr Aloke Chatterjee, (Lawrence Berkeley National Laboratory) and including Drs Les Braby, John Ford (Texas A&M) and Kathy Held (MGH Boston), which was developing an integrated theoretical and experimental model of the radiation-induced bystander response. Our part of the study has been to determine the effectiveness of soft X-rays at inducing chromosomal damage under conditions of direct and bystander exposure. The aim was to compare this with the effectiveness of the low energy 60 kV electron microbeam available at Texas A&M. Previous studies have been performed withmore » primary human fibroblasts measuring micronuclei formation to determine the relative yields of direct versus bystander mediated micronuclei formation after cells were individually irradiated utilizing our novel focused soft X-ray microprobe, which is capable of producing localized submicron beams of carbon-K (278 eV) X-rays. Only a brief overview is given here as the study has been published in several papers. Our original hypothesis was to study yields of bystander-induced micronucleated cells in both wild-type and mutant fibroblast from mouse embryo fibroblasts. Difficulties with the level of background micronuclei in the MEFs prevented systematic studies of bystander responses in the laboratories involved in the collaboration. We then performed these studies with AG1522 primary human fibroblast cells using a siRNA approach developed by John Ford at Texas A&M to knock down DNA PKcs in the first instance. Our soft X-ray source has been in routine use for carbon-K X-rays and is now available with Aluminium-K (1.49 keV) and titanium-K (4.5 keV), although the dose-rate from titanium is still too low at present for most experiments, where large numbers of cells need to be exposed. A separately funded project developed a new soft X-ray microprobe which will give much greater flexibility for changing energies and giving high dose-rates for exposures (See DE-FG02-01ER63236). However, we performed pilot studies measuring bystander responses with titanium-K. To date we have performed studies with V79 cells measuring cell survival as an endpoint and are starting studies in our human fibroblasts to measure micronuclei yields. A significant bystander response is observed in the V79 cells under conditions where only a single cell within a population was irradiated either with carbon-K or titanium-K X-rays. Typically around 10% cell killing is observed under these conditions. These studies are now being extended to measure micronuclei yields in the AG1522 cells under direct and bystander conditions. Our work has suggested that the yield of micronuclei in fibroblasts exposed to soft X-rays may be reduced in comparison to conventional X-ray exposures (Prise et al., 2003). Although further studies are required to confirm this using a range of scoring times.« less

  14. FTIR Analysis of Aerogel Keystones from the Stardust Interstellar Dust Collector: Assessment of Terrestrial Organic Contamination and X-Ray Microprobe Beam Damage

    NASA Astrophysics Data System (ADS)

    Bechtel, H. A.; Allen, C.; Bajt, S.; Borg, J.; Brenker, F.; Bridges, J.; Brownlee, D. E.; Burchell, M.; Burghammer, M.; Butterworth, A. L.; Cloetens, P.; Davis, A. M.; Floss, C.; Flynn, G. J.; Frank, D.; Gainsforth, Z.; Grun, E.; Heck, P. R.; Hillier, J. K.; Hoppe, P.; Howard, L.; Huss, G. R.; Huth, J.; Kearsley, A.; King, A. J.; Lai, B.; Leitner, J.; Lemelle, L.; Leroux, H.; Nittler, L. R.; Ogliore, R. C.; Postberg, F.; Price, M. C.; Sandford, S. A.; Sans Tresseras, J. A.; Schmitz, S.; Schoonjans, T.; Silversmit, G.; Simionovici, A.; Srama, R.; Stadermann, F. J.; Stephan, T.; Stodolna, J.; Stroud, R. M.; Sutton, S. R.; Toucoulou, R.; Trieloff, M.; Tsou, P.; Tsuchiyama, A.; Tyliczszak, T.; Vekemans, B.; Vincze, L.; Westphal, A. J.; Zolensky, M. E.; 29,000 Stardust@Home Dusters

    2011-03-01

    More than 20 aerogel keystones, many of which contained candidates for interstellar dust, were extracted from the Stardust interstellar dust collector and examined with synchrotron FTIR spectromicroscopy.

  15. Zirconolites from Sri Lanka, South Africa and Brazil

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

    Ewing, R.C.; Haaker, R.F.; Headley, T.J.

    1981-01-01

    Zirconolites, CaZrTi/sub 2/O/sub 7/, from Sri Lanka and Pala Bora, South Africa, and a calzirtite, CaZr/sub 3/TiO/sub 9/, from Jacupiranga, Brazil, were examined using the electron microprobe, x-ray diffraction (annealing study), transmission electron microscopy, scanning electron microscopy and optical microscopy. The x-ray data indicate that all three zirconolites are metamict. Both Sri Lanka zirconolites are amorphous to the limits of resolution of the electron microscope (approx. 10 A). The Pala Bora zirconolite is largely amorphous but contains isolated domains (50 to 200 A) of crystalline material which may be the result of post-metamict recrystallization and alteration. The only other significantmore » evidence for chemical alteration was the lower ThO/sub 2/ concentration (1 to 2 weight percent) and slightly lower analytic totals for the rims of the Sri Lanka zirconolites. Upon annealing at 1130/sup 0/C for 5 hours, all three zirconolites recrystallized as microcrystalline aggregates. Refined unit cell parameters and volumes are consistent with published data for synthetic zirconolites. Both Sri Lanka zirconolites contain microvoids, spherical in shape, and 200 Angstroms to 2 microns in size. This porosity may be the result of helium accumulation arising from the decay of U and Th. The calzirtite was highly crystalline, exhibited no porosity, and was unchanged by the annealing treatment.« less

  16. The Race To X-ray Microbeam and Nanobeam Science

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

    Ice, Gene E; Budai, John D; Pang, Judy

    2011-01-01

    X-ray microbeams are an emerging characterization tool with transformational implications for broad areas of science ranging from materials structure and dynamics, geophysics and environmental science to biophysics and protein crystallography. In this review, we discuss the race toward sub-10 nm- x-ray beams with the ability to penetrate tens to hundreds of microns into most materials and with the ability to determine local (crystal) structure. Examples of science enabled by current micro/nanobeam technologies are presented and we provide a perspective on future directions. Applications highlighted are chosen to illustrate the important features of various submicron beam strategies and to highlight themore » directions of current and future research. While it is clear that x-ray microprobes will impact science broadly, the practical limit for hard x-ray beam size, the limit to trace element sensitivity, and the ultimate limitations associated with near-atomic structure determinations are the subject of ongoing research.« less

  17. Electron Microscopy and Analytical X-ray Characterization of Compositional and Nanoscale Structural Changes in Fossil Bone

    NASA Astrophysics Data System (ADS)

    Boatman, Elizabeth Marie

    The nanoscale structure of compact bone contains several features that are direct indicators of bulk tissue mechanical properties. Fossil bone tissues represent unique opportunities to understand the compact bone structure/property relationships from a deep time perspective, offering a possible array of new insights into bone diseases, biomimicry of composite materials, and basic knowledge of bioapatite composition and nanoscale bone structure. To date, most work with fossil bone has employed microscale techniques and has counter-indicated the survival of bioapatite and other nanoscale structural features. The obvious disconnect between the use of microscale techniques and the discernment of nanoscale structure has prompted this work. The goal of this study was to characterize the nanoscale constituents of fossil compact bone by applying a suite of diffraction, microscopy, and spectrometry techniques, representing the highest levels of spatial and energy resolution available today, and capable of complementary structural and compositional characterization from the micro- to the nanoscale. Fossil dinosaur and crocodile long bone specimens, as well as modern ratite and crocodile femurs, were acquired from the UC Museum of Paleontology. Preserved physiological features of significance were documented with scanning electron microscopy back-scattered imaging. Electron microprobe wavelength-dispersive X-ray spectroscopy (WDS) revealed fossil bone compositions enriched in fluorine with a complementary loss of oxygen. X-ray diffraction analyses demonstrated that all specimens were composed of apatite. Transmission electron microscopy (TEM) imaging revealed preserved nanocrystallinity in the fossil bones and electron diffraction studies further identified these nanocrystallites as apatite. Tomographic analyses of nanoscale elements imaged by TEM and small angle X-ray scattering were performed, with the results of each analysis further indicating that nanoscale structure is highly conserved in these four fossil specimens. Finally, the results of this study indicate that bioapatite can be preserved in even the most ancient vertebrate specimens, further supporting the idea that fossilization is a preservational process. This work also underlines the importance of using appropriately selected characterization and analytical techniques for the study of fossil bone, especially from the perspective of spatial resolution and the scale of the bone structural features in question.

  18. Isomorphism and solid solutions among Ag- and Au-selenides

    NASA Astrophysics Data System (ADS)

    Palyanova, Galina A.; Seryotkin, Yurii V.; Kokh, Konstantin A.; Bakakin, Vladimir V.

    2016-09-01

    Au-Ag selenides were synthesized by heating stoichiometric mixtures of elementary substances of initial compositions Ag2-xAuxSe with a step of х=0.25 (0≤х≤2) to 1050 °С and annealing at 500 °C. Scanning electron microscopy, optical microscopy, electron microprobe analysis and X-ray powder diffraction methods have been applied to study synthesized samples. Results of studies of synthesized products revealed the existence of three solid solutions with limited isomorphism Ag↔Au: naumannite Ag2Se - Ag1.94Au0.06Se, fischesserite Ag3AuSe2 - Ag3.2Au0.8Se2 and gold selenide AuSe - Au0.94Ag0.06Se. Solid solutions and AgAuSe phases were added to the phase diagram of Ag-Au-Se system. Crystal-chemical interpretation of Ag-Au isomorphism in selenides was made on the basis of structural features of fischesserite, naumannite, and AuSe.

  19. Trace Element Abundance Measurements on Cosmic Dust Particles

    NASA Technical Reports Server (NTRS)

    Flynn, George

    1996-01-01

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

  20. Composition, structure, and properties of iron-rich nontronites of different origins

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

    Palchik, N. A., E-mail: nadezhda@igm.nsc.ru; Grigorieva, T. N.; Moroz, T. N.

    2013-03-15

    The composition, structure, and properties of smectites of different origins have been studied by X-ray diffraction, IR spectroscopy, scanning electron microscopy, and microprobe analysis. The results showed that nontronites of different origins differ in composition, properties, morphology, and IR spectroscopic characteristics. Depending on the degree of structural order and the negative charge of iron-silicate layers in nontronites, the shift of the 001 reflection to smaller angles as a result of impregnation with ethylene glycol (this shift is characteristic of the smectite group) occurs differently. The calculated values of the parameter b (from 9.11 to 9.14A) are valid for the extrememore » terms of dioctahedral smectite representatives: nontronites.« less

  1. Arizona porphyry copper/hydrothermal deposits II: Crystal structure of ajoite, (K + Na)3Cu20Al3Si29O76(OH)16⋅∼8H2O

    PubMed Central

    Pluth, Joseph J.; Smith, Joseph V.

    2002-01-01

    A crystal from the type locality Ajo, AZ, yielded just enough intensity from streaked diffractions using synchrotron x-rays at the Advanced Photon Source to solve the crystal structure with composition (K + Na)3Cu20Al3Si29O76(OH)16⋅∼8H2O; triclinic, P1̄, a = 13.634(5) Å, b = 13.687(7), c = 14.522(7), α = 110.83(1)°, β = 107.21(1), γ = 105.68(1); refined to a final R = 12.5%. Electron microprobe analysis yielded a similar chemical composition that is slightly different from the combined chemical and electron microprobe analyses in the literature. The ajoite structure can be described as a zeolitic octahedral-tetrahedral framework that combines the alternate stacking of edge-sharing octahedral CuO6 layers and curved aluminosilicate layers and strings. Channels bounded by elliptical 12-rings and circular 8-rings of tetrahedra contain (K and Na) ions and water. The Al atoms occupy some of the Si tetrahedral sites. Each Cu atom has near-planar bonds to four oxygen atoms plus two longer distances that generate a distorted octahedron. Valence bond estimates indicate that 8 oxygen atoms of 46 are hydroxyl. Only one alkali atom was located in distorted octahedral coordination, and electron microprobe analyses indicate K and Na as major substituents. The water from chemical analysis presumably occurs as disordered molecules of zeolitic type not giving electron density from diffraction. The high R factor results from structural disorder and many weak intensities close to detection level. The crystal chemistry is compared with shattuckite, Cu5(SiO3)4(OH)2, and planchéite, Cu8Si8O22(OH)4⋅H2O, both found in oxidized copper deposits of Arizona but only the former directly with ajoite. PMID:12177404

  2. Arizona porphyry copper/hydrothermal deposits II: crystal structure of ajoite, (K + Na)3Cu20Al3Si29O76(OH)16*~8H2O.

    PubMed

    Pluth, Joseph J; Smith, Joseph V

    2002-08-20

    A crystal from the type locality Ajo, AZ, yielded just enough intensity from streaked diffractions using synchrotron x-rays at the Advanced Photon Source to solve the crystal structure with composition (K + Na)3Cu20Al3Si29O76(OH)16* approximately 8H2O; triclinic, P1, a = 13.634(5) A, b = 13.687(7), c = 14.522(7), alpha = 110.83(1) degrees, beta = 107.21(1), gamma = 105.68(1); refined to a final R = 12.5%. Electron microprobe analysis yielded a similar chemical composition that is slightly different from the combined chemical and electron microprobe analyses in the literature. The ajoite structure can be described as a zeolitic octahedral-tetrahedral framework that combines the alternate stacking of edge-sharing octahedral CuO6 layers and curved aluminosilicate layers and strings. Channels bounded by elliptical 12-rings and circular 8-rings of tetrahedra contain (K and Na) ions and water. The Al atoms occupy some of the Si tetrahedral sites. Each Cu atom has near-planar bonds to four oxygen atoms plus two longer distances that generate a distorted octahedron. Valence bond estimates indicate that 8 oxygen atoms of 46 are hydroxyl. Only one alkali atom was located in distorted octahedral coordination, and electron microprobe analyses indicate K and Na as major substituents. The water from chemical analysis presumably occurs as disordered molecules of zeolitic type not giving electron density from diffraction. The high R factor results from structural disorder and many weak intensities close to detection level. The crystal chemistry is compared with shattuckite, Cu5(SiO3)4(OH)2, and planchéite, Cu8Si8O22(OH)4.H2O, both found in oxidized copper deposits of Arizona but only the former directly with ajoite.

  3. 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

  4. Old friends in a new light: “SnSb” revisited

    NASA Astrophysics Data System (ADS)

    Norén, Lasse; Withers, Ray L.; Schmid, Siegbert; Brink, Frank J.; Ting, Valeska

    2006-02-01

    The binary pnictide 'SnSb' has been re-investigated using a combination of X-ray, synchrotron and electron diffraction as well as electron microprobe analysis. Its structure was found to be incommensurately modulated with an underlying rhombohedral parent structure of space group symmetry R3¯m (No. 166), unit cell parameters a=b=4.3251(4) Å, c=5.3376(6) Å in the hexagonal setting. The incommensurate primary modulation wave vector q=1.3109(9)ch* and the superspace group symmetry is R3¯m (0, 0, ˜1.311) (No. 166.1). The refinement of the incommensurate structure indicates that the satellite reflections arise from displacive shifts of presumably essentially pure Sn and Sb layers along the hexagonal c-axis, with increasing distance between the Sn-layers and decreasing distance between the Sb layers.

  5. Ultrastructure of selected struvite-containing urinary calculi from dogs.

    PubMed

    Domingo-Neumann, R A; Ruby, A L; Ling, G V; Schiffman, P S; Johnson, D L

    1996-09-01

    To elucidate the ultrastructural details of struvite-containing urinary calculi from dogs. 38 specimens were selected from a collection of approximately 13,000 canine urinary calculi: 18 of these were composed entirely of struvite, and 20 consisted of struvite and calcium phosphate (apatite). Qualitative and quantitative analyses of specimens included use of plain and polarized light microscopy, x-ray diffractometry, scanning electron microscopy with backscattered electron imagery, x-ray fluorescence scans, and electron microprobe analysis. 4 textural types were recognized among struvite calculi, and 4 textural types of struvite-apatite calculi were described. Evidences of calculus dissolution were described from 4 calculi studied. The presence of small, well interconnected primary pores in struvite-containing urinary calculi from dogs appears to be a significant factor in determining the possible interaction of calculi with changes in the urine composition. The progress of dissolution from the calculus surface to the calculus interior appears to be largely affected by the primary porosity originally present between crystals forming the calculus framework. Apatite was observed to be more resistant to dissolution than struvite. The prevalence of fine concentric laminations having low porosity, and the common occurrence of apatite among struvite-containing urinary calculi from dogs may be 2 reasons why the efficacy of dietary and medicinal manipulations in dissolving urinary calculi is greater among cats than it is among dogs.

  6. Microprobe studies of microtomed particles of white druse salts in shergottite EETA 79001

    NASA Technical Reports Server (NTRS)

    Lindstrom, D. J.

    1991-01-01

    The white druse material in Antarctic shergottite EETA 79001 has attracted much attention as a possible sample fo Martian aqueous deposits. Instrumental Neutron Activation Analysis (INAA) was used to determine trace element analyses of small particles of this material obtained by handpicking of likely grains from broken surfaces of the meteorite. Electron microprobe work was attempted on grain areas as large as 150x120 microns. Backscattered electron images show considerable variations in brightness, and botryoidal structures were observed. Microprobe analyses showed considerable variability both within single particles and between different particles. Microtomed surfaces of small selected particles were shown to be very useful in obtaining information on the texture and composition of rare lithologies like the white druse of EETA 79001. This material is clearly heterogeneous on all distance scales, so a large number of further analyses will be required to characterize it.

  7. De-MA: a web Database for electron Microprobe Analyses to assist EMP lab manager and users

    NASA Astrophysics Data System (ADS)

    Allaz, J. M.

    2012-12-01

    Lab managers and users of electron microprobe (EMP) facilities require comprehensive, yet flexible documentation structures, as well as an efficient scheduling mechanism. A single on-line database system for managing reservations, and providing information on standards, quantitative and qualitative setups (element mapping, etc.), and X-ray data has been developed for this purpose. This system is particularly useful in multi-user facilities where experience ranges from beginners to the highly experienced. New users and occasional facility users will find these tools extremely useful in developing and maintaining high quality, reproducible, and efficient analyses. This user-friendly database is available through the web, and uses MySQL as a database and PHP/HTML as script language (dynamic website). The database includes several tables for standards information, X-ray lines, X-ray element mapping, PHA, element setups, and agenda. It is configurable for up to five different EMPs in a single lab, each of them having up to five spectrometers and as many diffraction crystals as required. The installation should be done on a web server supporting PHP/MySQL, although installation on a personal computer is possible using third-party freeware to create a local Apache server, and to enable PHP/MySQL. Since it is web-based, any user outside the EMP lab can access this database anytime through any web browser and on any operating system. The access can be secured using a general password protection (e.g. htaccess). The web interface consists of 6 main menus. (1) "Standards" lists standards defined in the database, and displays detailed information on each (e.g. material type, name, reference, comments, and analyses). Images such as EDS spectra or BSE can be associated with a standard. (2) "Analyses" lists typical setups to use for quantitative analyses, allows calculation of mineral composition based on a mineral formula, or calculation of mineral formula based on a fixed amount of oxygen, or of cation (using an analysis in element or oxide weight-%); this latter includes re-calculation of H2O/CO2 based on stoichiometry, and oxygen correction for F and Cl. Another option offers a list of any available standards and possible peak or background interferences for a series of elements. (3) "X-ray maps" lists the different setups recommended for element mapping using WDS, and a map calculator to facilitate maps setups and to estimate the total mapping time. (4) "X-ray data" lists all x-ray lines for a specific element (K, L, M, absorption edges, and satellite peaks) in term of energy, wavelength and peak position. A check for possible interferences on peak or background is also possible. Theoretical x-ray peak positions for each crystal are calculated based on the 2d spacing of each crystal and the wavelength of each line. (5) "Agenda" menu displays the reservation dates for each month and for each EMP lab defined. It also offers a reservation request option, this request being sent by email to the EMP manager for approval. (6) Finally, "Admin" is password restricted, and contains all necessary options to manage the database through user-friendly forms. The installation of this database is made easy and knowledge of HTML, PHP, or MySQL is unnecessary to install, configure, manage, or use it. A working database is accessible at http://cub.geoloweb.ch.

  8. Thermoelectric Inhomogeneities in (Ag(sub 1-y)SbTe2)(sub x)(PbTe)(sub 1-x)

    NASA Technical Reports Server (NTRS)

    Snyder, G. Jeffrey; Chen, Nancy; Gascoin, Franck; Mueller, Eckhard; Karpinski, Gabriele; Stiewe, Christian

    2006-01-01

    A document presents a study of why materials of composition (Ag1 ySbTe2)0.05 (PbTe)0.95 [0< or = y < or = 1] were previously reported to have values of the thermoelectric figure of merit [ZT (where Z = alpha(sup 2)/rk, alpha is the Seebeck coefficient, r is electrical resistivity, k is thermal conductivity, and T is absolute temperature)] ranging from <1 to >2. In the study, samples of (AgSbTe2)0.05(PbTe)0.95, (Ag0.67SbTe2)0.05 (PbTe)0.95, and (Ag0.55SbTe2)0.05(PbTe)0.95 were prepared by melting followed, variously, by slow or rapid cooling. Analyses of these samples by x-ray diffraction, electron microscopy, and scanning-microprobe measurements of the Seebeck coefficient led to the conclusion that these materials have a multiphase character on a scale of the order of millimeters, even though they appear homogeneous in x-ray diffraction and electron microscopy. The Seebeck measurements showed significant variations, including both n-type and p-type behavior in the same sample. These variations were found to be consistent with observed variations of ZT. The rapidly quenched samples were found to be less inhomogeneous than were the furnace-cooled ones; hence, rapid quenching was suggested as a basis of research on synthesizing more nearly uniform high-ZT samples.

  9. Beamline 10.3.2 at ALS: a hard X-ray microprobe for environmental and materials sciences.

    PubMed

    Marcus, Matthew A; MacDowell, Alastair A; Celestre, Richard; Manceau, Alain; Miller, Tom; Padmore, Howard A; Sublett, Robert E

    2004-05-01

    Beamline 10.3.2 at the ALS is a bend-magnet line designed mostly for work on environmental problems involving heavy-metal speciation and location. It offers a unique combination of X-ray fluorescence mapping, X-ray microspectroscopy and micro-X-ray diffraction. The optics allow the user to trade spot size for flux in a size range of 5-17 microm in an energy range of 3-17 keV. The focusing uses a Kirkpatrick-Baez mirror pair to image a variable-size virtual source onto the sample. Thus, the user can reduce the effective size of the source, thereby reducing the spot size on the sample, at the cost of flux. This decoupling from the actual source also allows for some independence from source motion. The X-ray fluorescence mapping is performed with a continuously scanning stage which avoids the time overhead incurred by step-and-repeat mapping schemes. The special features of this beamline are described, and some scientific results shown.

  10. Preparation and Thermoelectric Properties of Semiconcucting Zn(sub 4) Sb(sub 3)

    NASA Technical Reports Server (NTRS)

    Caillat, T.; Fleurial, J. P.; Barshchevsky, A.

    1996-01-01

    Hot-pressed samples fothe semiconducting compound Beta - Zn(sub 4) Sb(sub 3) were prepared and characterized by x-ray and microprobe analysis. Some physical properties of Beta - Zn(sub 4) Sb(sub 3) were determined and its thermoelectric properties measured between room temperature and 650K.

  11. Vanadium Geochemistry of Oil Sands Fluid Petroleum Coke.

    PubMed

    Nesbitt, Jake A; Lindsay, Matthew B J

    2017-03-07

    Vanadium has previously been linked to elevated toxicity of leachates derived from oil sands petroleum coke. However, geochemical controls on V mobility within coke deposits remain poorly constrained. Detailed examinations of porewater and solid-phase V geochemistry were therefore performed on oil sands fluid petroleum coke deposits in Alberta, Canada. Sample collection focused on both active and reclaimed deposits, which contained more than 3 × 10 7 m 3 of fluid petroleum coke. Dissolved V concentrations were highest (up to 3.0 mg L -1 ) immediately below the water table but decreased rapidly with increasing depth. This trend corresponded to a transition from mildly acidic (pH 6-7) and oxic conditions to mildly alkaline (pH 7-8.5) and anoxic conditions. Scanning electron microscopy (SEM), electron microprobe analysis (EMPA), and micro-X-ray fluorescence (μXRF) mapping revealed coke particles exhibited an internal structure characterized by successive concentric layers. The outer margins of these layers were characterized by elevated V, Fe, Si, and Al concentrations, indicating the presence of inorganic phases. Micro-X-ray absorption near-edge structure (μXANES) spectroscopy revealed that V speciation was dominated by V(IV) porphyrins except at outer margins of layers, where octahedrally coordinated V(III) was a major component. Minor to trace V(V) was also detected within fluid petroleum coke particles.

  12. GeoSoilEnviroCARS: A National User Facility for Synchrotron Radiation Research

    NASA Astrophysics Data System (ADS)

    Rivers, M. L.; Sutton, S. R.

    2002-12-01

    GeoSoilEnviroCARS (GSECARS) is a national user facility for frontier research in the earth sciences using synchrotron radiation at the Advanced Photon Source, Argonne National Laboratory. GSECARS provides earth scientists with access to the high-brilliance hard x-rays from this third-generation synchrotron light source. Both an undulator and a bending magnet beamline are available. All principal synchrotron-based analytical techniques in demand by earth scientists are being brought to bear on earth science problems: (1) high-pressure/high-temperature crystallography and spectroscopy using the diamond anvil cell; (2) high-pressure/high-temperature crystallography using the large-volume press; (3) powder, single crystal and interface diffraction; (4) inelastic x-ray scattering; (5) x-ray absorption fine structure (XAFS) spectroscopy; (6) x-ray fluorescence microprobe analysis; and (7) microtomography. The major instrumentation includes 250 and 1000 MN multianvil presses, a double-sided laser heating system, a large general-purpose 5-circle diffractometer, a focused microprobe, and a Raman laboratory. A proposal-based system for beamtime allocation, open to all earth scientists, has been in place since Fall, 1998. Since then, over 450 beamtime proposals have been received and more than 320 outside users have conducted experiments at GSECARS. The research conducted by these investigators has resulted in more than 170 publications. The unique capabilities of the APS and GSECARS have allowed groundbreaking experiments to be conducted. These include: (1) phase transformations in the Mg-Si-O system at mantle conditions; (2) structure of hydrated a-Al2O3 surfaces; (3) alloying properties of silicon in the Earth's core; (4) dynamics of iron-rich melt segregation from silicates during core formation; (5) electronic spin state of FeO at high pressure and temperature; (6) elastic wave velocities of mantle minerals at lower mantle conditions; (7) copper partitioning and speciation in natural hydrothermal fluids; and (8) mechanisms of arsenic sequestration at a Superfund site. The GSECARS mission is to provide a research environment where users receive expert assistance in planning and conducting experiments, and in analyzing data. The facility operation is funded by the NSF EAR Instrumentation and Facilities program and the DOE Geosciences program. Major instrumentation was also provided by the W.M. Keck Foundation. Information and applications for beam time can be found at http://gsecars.org.

  13. Macrosegregation of GeSi Alloys Grown in a Static Magnetic Field

    NASA Technical Reports Server (NTRS)

    Ritter, T. M.; Volz, M. P.; Cobb, S. D.; Szofran, F. R.

    1999-01-01

    Axial and radial macrosegregation profiles have been determined for GeSi alloy crystals grown by the vertical Bridgman technique. An axial 5 Tesla magnetic field was applied to several samples during growth to decrease the melt velocities by means of the Lorentz force. Compositions were measured with either energy dispersive X-ray spectroscopy (EDS) on a scanning electron microscope (SEM) or by wavelength dispersive X-ray spectroscopy (WDS) on a microprobe. The crystals were processed in graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN) ampoules, which produced various solid-liquid interface shapes during solidification. Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. Possible explanations for the apparent insufficiency of the magnetic field to achieve diffusion controlled growth conditions are discussed.

  14. Post-flight analyses of the crystals from the M0003-14 quartz crystal microbalance experiment

    NASA Technical Reports Server (NTRS)

    Stuckey, W. K.; Radhakrishnan, G.; Wallace, D.

    1993-01-01

    Quartz Crystal Microbalances constructed by QCM Research were flown on the leading and trailing edges of LDEF as one of the sub-experiments of M0003. Response of the crystals coated with 150 A of In2O3 was recorded during the first 424 days of the mission. A second QCM with crystals coated with 150 A of ZnS was also flown but not monitored. After the flight, the QCM's were disassembled and analyzed in The Aerospace Corporation laboratories. The samples included the crystals from the leading and trailing edge samples of both types of coatings along with the reference crystals, which were inside the QCM housing. Analyses were performed by scanning electron microscopy, energy dispersive x-ray analyses, x-ray photoelectron spectroscopy, ion microprobe mass analysis, and reflectance spectroscopy in the infrared and UV/visible regions. The crystals are contaminated predominantly with silicone compounds. The contamination is higher on the leading edge than on the trailing edge and higher on the exposed crystals than on the reference crystals.

  15. Geochemistry and origin of regional dolomites. Final report

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

    Hanson, G.N.; Meyers, W.J.

    1995-05-01

    The main goal of our research on dolomites has been to better understand the composition of the fluids and processes of the fluid-rock interaction responsible for the formation of massive dolostones occurring over regional scales within sedimentary sequences. Understanding the timing of dolomitization, the fluids responsible for the dolomitization and the timing of the development of porosity has major economic ramifications in that dolomites are major oil reservoirs often having better reservoir properties than associated limestones. Our approach has been to apply trace element, major element, petrographic, crystallographic, stable isotope and radiogenic isotope systems to test models for the originsmore » of dolomites and to give information that may allow us to develop new models. Fluid compositions and processes are evaluated through the use of numerical models which we have developed showing the simultaneous evolution of the trace element and isotope systems during dolomitization. Our research has included the application of B, O, C, Sr, Nd and Pb isotope systematics and the trace elements Mn, Fe St, rare earth elements, Rb, Ba, U, Th, Pb, Zn, Na, Cl, F and SO{sub 4}{sup 2-}. Analyses are possible on individual cements or dolomite types using micro-sampling or microprobe techniques. The microprobe techniques used include synchrotron X-ray microprobe analysis at Brookhaven National Laboratory or electron microprobe at Stony Brook. Lack of a modern analogue for ancient massive dolostones has limited the application of the uniformitarian concept to developing models for the ancient regional dolostones. In addition it has not been possible to synthesize dolomite in the laboratory under conditions similar to the sedimentary or diagenetic possible environments in which the dolomites must have formed.« less

  16. Phase diagram and electrical behavior of silicon-rich iridium silicide compounds

    NASA Technical Reports Server (NTRS)

    Allevato, C. E.; Vining, Cronin B.

    1992-01-01

    The iridium-silicon phase diagram on the silicon-rich side was investigated by means of X-ray powder diffraction, density, differential thermal analysis, metalography, microprobe analysis, and electrical resistivity. Attempts were made to prepare eight previously reported silicon-rich iridium silicide compounds by arc melting and Bridgman-like growth. However, microprobe analysis identified only four distinct compositions: IrSi, Ir3Si4, Ir3Si5 and IrSi sub about 3. The existence of Ir4Si5 could not be confirmed in this study, even though the crystal structure has been previously reported. Differential thermal analysis (DTA) in conjunction with X-ray powder diffraction confirm polymorphism in IrSi sub about 3, determined to have orthorhombic and monoclinic unit cells in the high and low temperature forms. A eutectic composition alloy of 83 +/- 1 atomic percent silicon was observed between IrSi sub about 3 and silicon. Ir3Si4 exhibits distinct metallic behavior while Ir3Si5 is semiconducting. Both and IrSi and IrSi sub about 3 exhibit nearly temperature independent electrical resistivities on the order of 5-10 x 10 exp -6 ohms-m.

  17. High-resolution EPMA X-ray images of mother liquid inclusions in a Pd2Ga single crystal

    NASA Astrophysics Data System (ADS)

    Müller, D.; Schwerin, J.; Gille, P.; Fehr, K. T.

    2014-03-01

    During crystal growth from solution inclusions of different compositions were trapped at the rim of a Pd2Ga single crystal. Their fine-grained (< 5 μm) internal structure demands special requirements for electron microprobe analysis, realized by low-voltage (5 keV) element mapping applying a step size of 0.138 μm for each pixel. It can be shown, that these inclusions represent an isolated chemical system, and that crystallisation upon cooling follows the expected thermodynamic phase relations. Thus the final composition in the centre of the inclusion consists of a small-scale mixture of PdGa and Pd5Ga3 evolved out of a solid-solid decomposition of Pd5Ga4.

  18. Crystalline solution series and order-disorder within the natrolite mineral group

    USGS Publications Warehouse

    Ross, M.; Flohr, M.J.K.; Ross, D.R.

    1992-01-01

    Electron microprobe and X-ray analyses were made of natrolite, tetranatrolite, gonnardite, and thomsonite from the Magnet Cove alkaline igneous complex, Arkansas, and of selected specimens from the U.S. National Museum. This information and data from the literature indicate that natrolite, mesolite, scolecite, edingtonite, and tetraedingtonite show only small deviations from the ideal stoichiometry. In contrast, gonnardite, tetranatrolite, and thomsonite show large deviations from the ideal end-member compositions and compose three crystalline series. The structures of the natrolite minerals are defined by combining each of the three types of framework structures with various combinations of channel-occupying polyhedra. Various polysomatic series can be constructed by combining slices of two basic structures to form new hybrid structures. -from Authors

  19. Electron-probe microanalysis of light elements in coal and other kerogen

    USGS Publications Warehouse

    Bustin, R.M.; Mastalerz, Maria; Raudsepp, M.

    1996-01-01

    Recent advances in electron microprobe technology including development of layered synthetic microstructures, more stable electronics and better matrix-correction programs facilitated routine microanalysis of the light elements in coal. Utilizing an appropriately equipped electron microprobe with suitable standards, it is now possible to analyze directly the light elements (C, O and N, if abundant) in coal macerals and other kerogen. The analytical results are both accurate compared to ASTM methods and highly precise, and provide an opportunity to access the variation in coal chemistry at the micrometre scale. Our experiments show that analyses using a 10 kV accelerating voltage and 10 nA beam current yield the most reliable data and result in minimum sample damage and contamination. High sample counts were obtained for C, O and N using a bi-elemental nickel-carbon pseudo-crystal (2d = 9.5 nm) as an analyzing crystal. Vitrinite isolated from anthracite rank coal proves the best carbon standard and is more desirable than graphite which has higher porosity, whereas lower rank vitrinite is too heterogeneous to use routinely as a standard. Other standards utilized were magnesite for oxygen and BN for nitrogen. No significant carbon, oxygen or nitrogen X-ray peak shifts or peak-shape changes occur between standards and the kerogen analyzed. Counting rates for carbon and oxygen were found to be constant over a range of beam sizes and currents for counting times up to 160 s. Probe-determined carbon and oxygen contents agree closely with those reported from ASTM analyses. Nitrogen analyses compare poorly to ASTM values which probably is in response to overlap between the nitrogen Ka peak with the carbon K-adsorption edge and the overall low nitrogen content of most of our samples. Our results show that the electron microprobe technique provides accurate compositional data for both minor and major elements in coal without the necessity and inherent problems associated with mechanically isolating macerals. Studies to date have demonstrated the level of compositional variability within and between macerals in suites of Canadian coals.

  20. Growth Structure and Properties of Gradient Nanocrystalline Coatings of the Ti-Al-Si-Cu-N System

    NASA Astrophysics Data System (ADS)

    Ovchinnikov, S. V.; Pinzhin, Yu. P.

    2016-10-01

    Methods of electron microprobe analysis, X-ray structure analysis and electron microscopy were used to study the element composition and features of the structure-phase, elastic stress state of nanocrystalline coatings of the Ti- Al- Si- Cu- N system with gradient of copper concentration across their thickness. The authors established the effects of element composition modification, non-monotonous behavior of the lattice constant of alloyed nitride and rise in the bending-torsion value of the crystalline lattice in individual nanocrystals to values of around 400 degrees/μm with increase in copper concentration, whereas the sizes of alloyed nitride crystals remained practically unchanged. Mechanical (hardness), adhesion and tribological properties of coatings were examined. Comparative analysis demonstrates higher values of adhesion characteristics in the case of gradient coatings of the Ti- Al- Si- Cu- N system than in the case of single-layer (with constant element concentration) analogues.

  1. Radiative properties of advanced spacecraft heat shield materials

    NASA Technical Reports Server (NTRS)

    Cunnington, G. R.; Funai, A. I.; Mcnab, T. K.

    1983-01-01

    Experimental results are presented to show the effects of simulated reentry exposure by convective heating and by radiant heating on spectral and total emittance of statically oxidized Inconel 617 and Haynes HS188 superalloys to 1260 K and a silicide coatea (R512E) columbium 752 alloy to 1590 K. Convective heating exposures were conducted in a supersonic arc plasma wind tunnel using a wedge-shaped specimen configuration. Radiant tests were conducted at a pressure of .003 atmospheres of dry air at a flow velocity of several meters per second. Convective heating specimens were subjected to 8, 20, and 38 15-min heating cycles, and radiant heating specimens were tested for 10, 20, 50, and 100 30-min heating cycles. Changes in radiative properties are explained in terms of changes in composition resulting from simulated reentry tests. The methods used to evaluate morphological, compositional and crystallographic changes include: Auger electron spectroscopy; scanning electron microscopy; X-ray diffraction analysis; and electron microprobe analysis.

  2. Oxidative dissolution potential of biogenic and abiogenic TcO 2 in subsurface sediments

    NASA Astrophysics Data System (ADS)

    Fredrickson, James K.; Zachara, John M.; Plymale, Andrew E.; Heald, Steve M.; McKinley, James P.; Kennedy, David W.; Liu, Chongxuan; Nachimuthu, Ponnusamy

    2009-04-01

    Technetium-99 (Tc) is an important fission product contaminant associated with sites of nuclear fuels reprocessing and geologic nuclear waste disposal. Tc is highly mobile in its most oxidized state [Tc(VII)O4-] and less mobile in the reduced form [Tc(IV)O 2· nH 2O]. Here we investigate the potential for oxidation of Tc(IV) that was heterogeneously reduced by reaction with biogenic Fe(II) in two sediments differing in mineralogy and aggregation state; unconsolidated Pliocene-age fluvial sediment from the upper Ringold (RG) Formation at the Hanford Site and a clay-rich saprolite from the Field Research Center (FRC) background site on the Oak Ridge Site. Both sediments contained Fe(III) and Mn(III/IV) as redox active phases, but FRC also contained mass-dominant Fe-phyllosilicates of different types. Shewanella putrefaciens CN32 reduced Mn(III/IV) oxides and generated Fe(II) that was reactive with Tc(VII) in heat-killed, bioreduced sediment. After bioreduction and heat-killing, biogenic Fe(II) in the FRC exceeded that in RG by a factor of two. More rapid reduction rates were observed in the RG that had lower biogenic Fe(II), and less particle aggregation. EXAFS measurements indicated that the primary reduction product was a TcO 2-like phase in both sediments. The biogenic redox product Tc(IV) oxidized rapidly and completely in RG when contacted with air. Oxidation, in contrast, was slow and incomplete in the FRC, in spite of similar molecular scale speciation of Tc compared to RG. X-ray microprobe, electron microprobe, X-ray absorption spectroscopy, and micro X-ray diffraction were applied to the whole sediment and isolated Tc-containing particles. These analyses revealed that non-oxidizable Tc(IV) in the FRC existed as complexes with octahedral Fe(III) within intra-grain domains of 50-100 μm-sized, Fe-containing micas presumptively identified as celadonite. The markedly slower oxidation rates in FRC as compared to RG were attributed to mass-transfer-limited migration of O 2 into intra-aggregate and intraparticle domains where Tc(IV) existed; and the formation of unique, oxidation-resistant, intragrain Tc(IV)-Fe(III) molecular species.

  3. Electron Microprobe Measurements of Nitrogen in SiC

    NASA Astrophysics Data System (ADS)

    Ross, K.

    2007-12-01

    Methods have been developed for the measurement of low abundances of nitrogen in SiC films. These techniques were developed for measurements of synthetic thin-film samples prepared by materials scientists but the technique can also be applied to natural SiC grains in meteorites. One problem associated with measuring nitrogen at low abundance levels is the low count rates due to strong absorption of the nitrogen signal in the matrix material. In thin film samples, (SiC deposited on elemental Si) it is preferable to limit x-ray production and emission to the overlayer. This eliminates the need for data reduction using thin-film methods. Thin film data reduction is inevitably less accurate than bulk material data reduction methods. In order to limit x-ray emission to the film layer, data has been collected at 5 kV and 3.5 kV accelerating voltage (depending on film thickness estimates provided by scientists who prepared these samples). These low beam energies also promote production of x-rays in the shallow region of the samples, and this minimizes strong absorption, leading to more abundant nitrogen x-ray detection, which improves counting statistics and overall precision. The CASINO monte carlo modeling program was used to model electron penetration and x-ray production as a function of beam energy and depth in the sample in order to ensure that the excited volume is limited to the film. The beam was set to 200 nA beam current. This high beam current also improves counting statistics by providing more abundant count rates. One drawback of these beam conditions is the limited spatial resolution provided. In our Cameca probe, a 5 kV, 200 nA beam is approximately 10 microns in diameter. SiC samples and standard were not carbon coated (they are conducting). AlN was used as the nitrogen standard. These films contained 0.3 to 0.7 wt. per cent nitrogen, with analytical uncertainties in the range of 10-20 per cent relative errors. The Si:C ratios were very near 1:1 indicating that little if any Si signal originated in the substrate of the film.

  4. Isomorphism and solid solutions among Ag- and Au-selenides

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

    Palyanova, Galina A.; Seryotkin, Yurii V.; Novosibirsk State University

    Au-Ag selenides were synthesized by heating stoichiometric mixtures of elementary substances of initial compositions Ag{sub 2−x}Au{sub x}Se with a step of x=0.25 (0≤x≤2) to 1050 °C and annealing at 500 °C. Scanning electron microscopy, optical microscopy, electron microprobe analysis and X-ray powder diffraction methods have been applied to study synthesized samples. Results of studies of synthesized products revealed the existence of three solid solutions with limited isomorphism Ag↔Au: naumannite Ag{sub 2}Se – Ag{sub 1.94}Au{sub 0.06}Se, fischesserite Ag{sub 3}AuSe{sub 2} - Ag{sub 3.2}Au{sub 0.8}Se{sub 2} and gold selenide AuSe - Au{sub 0.94}Ag{sub 0.06}Se. Solid solutions and AgAuSe phases were added tomore » the phase diagram of Ag-Au-Se system. Crystal-chemical interpretation of Ag-Au isomorphism in selenides was made on the basis of structural features of fischesserite, naumannite, and AuSe. - Highlights: • Au-Ag selenides were synthesized. • Limited Ag-Au isomorphism in the selenides is affected by structural features. • Some new phases were introduced to the phase diagram Ag-Au-Se.« less

  5. Effect of co-site dilution on the magnetism of RCo5 (R = Gd, Y) compounds

    NASA Astrophysics Data System (ADS)

    Nikitin, S. A.; Bogdanov, A. E.; Morozkin, A. V.; Knotko, A. V.; Yapaskurt, V. O.; Ovchenkova, I. A.; Smirnov, A. V.; Nirmala, R.; Quezado, S.; Malik, S. K.

    2018-03-01

    The magnetic and magnetocaloric properties of the RCo5‑x Ga x (R = Gd, Y; x = 1, 1.5, 1.6, 1.7) compounds have been studied. X-ray and electron microprobe analysis show that the samples are single phase and crystallize in the hexagonal CaCu5 - type structure (space group P6/mmm, N 191, hP6). The magnetic properties have been studied from 2 to 400 K under magnetic fields in the region of 1 to 140 kOe. With increasing Ga amount the magnetic ordering temperature decreases rapidly. The increase in Ga concentration leads to the reduction of the magnetic moment of Co sublattice and the Curie temperature. It has been found that the paramagnetic susceptibility follows the Néel-type law for GdCo5‑x Ga x (x = 1.5, 1.6, 1.7) and the Curie-Weiss law for YCo3.3Ga1.7. The molecular field coefficients and sublattice magnetizations were determined on a basis of the Néel theory and experimental data. The magnetocaloric effect and refrigerant capacity have been estimated over a wide temperature range of 10–350 K.

  6. Sulfides from Martian and Lunar Basalts: Comparative Chemistry for Ni Co Cu and Se

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

    J Papike; P Burger; C Shearer

    2011-12-31

    Here Mars and Moon are used as 'natural laboratories' with Moon displaying lower oxygen fugacities ({approx}IW-1) than Mars ({approx}IW to FMQ). Moon has lower concentrations of Ni and Co in basaltic melts than does Mars. The major sulfides are troilite (FeS) in lunar basalts and pyrrhotite (Fe{sub 1-x}S) in martian basalts. This study focuses on the concentrations of Ni, Co, Cu, and Se. We chose these elements because of their geochemical importance and the feasibility of analyzing them with a combination of synchrotron X-ray fluorescence (SXRF) and electron microprobe (EPMA) techniques. The selenium concentrations could only be analyzed, at highmore » precision, with SXRF techniques as they are <150 ppm, similar to concentrations seen in carbonaceous chondrites and interplanetary dust particles (IDPs). Nickel and Co are in higher concentrations in martian sulfides than lunar and are higher in martian olivine-bearing lithologies than olivine-free varieties. The sulfides in individual samples show very large ranges in concentration (e.g., Ni ranges from 50 000 ppm to <5 ppm). These large ranges are mainly due to compositional heterogeneities within individual grains due to diffusion and phase separation. Electron microprobe wavelength-dispersive (WDS) mapping of Ni, Co, and Cu show the diffusion trajectories. Nickel and Co have almost identical diffusion trajectories leading to the likely nucleation of pentlandite (Ni,Co,Fe){sub 9}S{sub 8}, and copper diffuses along separate pathways likely toward chalcopyrite nucleation sites (CuFeS{sub 2}). The systematics of Ni and Co in lunar and martian sulfides clearly distinguish the two parent bodies, with martian sulfides displaced to higher Ni and Co values.« less

  7. An experimental, low-cost, silicon slurry/aluminide high-temperature coating for superalloys

    NASA Technical Reports Server (NTRS)

    Young, S. G.; Deadmore, D. L.

    1979-01-01

    A duplex silicon-slurry/aluminide coating has been developed and cyclically tested in Mach 1 combustion gases for oxidation and thermal fatigue resistance at 1093 C and in Mach 0.3 gases for hot-corrosion resistance at 900 C. The base-metal superalloys were VIA and B-1900. The coated B-1900 specimens performed much better in oxidation than similar specimens coated with aluminides and almost as well as the more-expensive Pt-Al and MCrAlY (where M is Ni and/or Co) coatings deposited by the physical vapor deposition process. The coating also provided good hot-corrosion protection. Metallographic, X-ray, and electron microprobe studies were made to characterize the coating, determine failure mechanisms, and study some of the changes due to exposure.

  8. Electrochemical Atomic Layer Epitaxy of Thin Film CdSe

    NASA Astrophysics Data System (ADS)

    Pham, L.; Kaleida, K.; Happek, U.; Mathe, M. K.; Vaidyanathan, R.; Stickney, J. L.; Radevic, M.

    2002-10-01

    Electrochemical atomic layer epitaxy (EC-ALE) is a current developmental technique for the fabrication of compound semiconductor thin films. The deposition of elements making up the compound utilizes surface limited reactions where the potential is less than that required for bulk growth. This growth method offers mono-atomic layer control, allowing the deposition of superlattices with sharp interfaces. Here we report on the EC-ALE formation of CdSe thin films on Au and Cu substrates using an automated flow cell system. The band gap was measured using IR absorption and photoconductivity and found to be consistent with the literature value of 1.74 eV at 300K and 1.85 eV at 20K. The stoichiometry of the thin film was confirmed with electron microprobe analysis and x-ray diffraction.

  9. Pyroxenes in Serra de Mage - Cooling history in comparison with Moama and Moore County

    NASA Technical Reports Server (NTRS)

    Harlow, G. E.; Prinz, M.; Nehru, C. E.; Taylor, G. J.; Keil, K.

    1979-01-01

    Thin sections and single grains of pyroxenes from the Serra de Mage feldspar cumulate eucrites were studied by X-ray crystallography, electron microprobe and optical techniques. It was concluded that the pyroxene crystallized as pigeonite. On cooling augite was exsolved along (001) and inverted to hypersthene, with exsolution of (100) augite from hypersthene during continued slow cooling. The estimated original bulk composition of the pigeonite pyroxene is Wo10En51Fs39. The compositional data, textural relations, and existence of P2 sub 1 ca hypersthene suggest very low cooling (about 0.0004 deg C/year) below 800 deg. The Serra de Mage augite lamellae were found to be as thick or thicker than those of Moore County and Moama meteorites.

  10. Geology and geochemistry of the Arctic prospect, Ambler District, Alaska

    NASA Astrophysics Data System (ADS)

    Schmidt, J. M.

    The Arctic volcanogenic massive sulfide prospect is the largest known (40 million ton) deposit hosted by the low greenschist grade, latest Devonian Ambler Sequence of bimodal, basaltic and rhyolitic volcanic and volcanoclastic rocks, pelitic, graphitic and calcareous metasediments. Detailed field mapping, core logging, petrography, X-ray diffractometry, electron microprobe analyses and whole-rock major element analyses of hydrothermally altered rocks were used to determine the emplacement history and setting of sulfide deposition. Low greenschist grade metamorphism was essentially isochemical on a macroscopic scale, and preserved volcanic compositions, the major element chemistry of alteration and the compositions of individual metamorphic, alteration and relict igneous minerals. Mineralization at Arctic was formed along a synvolcanic fault in a tectonically and volcanically active basin within a rifted continental margin, possibly related to an actively spreading oceanic rift.

  11. Silver/oxygen depth profile in coins by using laser ablation, mass quadrupole spectrometer and X-rays fluorescence

    NASA Astrophysics Data System (ADS)

    Cutroneo, M.; Torrisi, L.; Caridi, F.; Sayed, R.; Gentile, C.; Mondio, G.; Serafino, T.; Castrizio, E. D.

    2013-05-01

    Silver coins belonging to different historical periods were investigated to determine the Ag/O atomic ratio depth profiles. Laser ablation has been employed to remove, in high vacuum, the first superficial layers of the coins. Mass quadrupole spectrometry has been used to detect the Ag and the O atomic elements vaporized from the coin surface. The depth profile allowed to determine the thickness of the oxidation layer indicating that, in general, it is high in old coins. A complementary technique, using scanning electron microscope and the associated XRF microprobe, have been devoted to confirm the measurements of Ag/O atomic ratio measured with the laser-coupled mass spectrometry. The oxidation layer thicknesses range between about 25 and 250 microns.

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

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Sutton, S. R.

    1989-01-01

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

  13. Speciation and characterization of arsenic in gold ores and cyanidation tailings using X-ray absorption spectroscopy

    USGS Publications Warehouse

    Paktunc, D.; Foster, A.; Heald, S.; Laflamme, G.

    2004-01-01

    The knowledge of mineralogy and molecular structure of As is needed to better understand the stability of As in wastes resulting from processing of gold ores. In this study, optical microscopy, scanning electron microscopy, electron microprobe, X-ray diffraction and X-ray absorption fine structure (XAFS) spectroscopy (including both XANES and EXAFS regimes) were employed to determine the mineralogical composition and local coordination environment of As in gold ores and process tailings from bench-scale tests designed to mimic a common plant practice. Arsenic-bearing minerals identified in the ores and tailings include iron (III) oxyhydroxides, scorodite (FeAsO4??2H2O), ferric arsenates, arseniosiderite (Ca2Fe3 (AsO4)3O2??3H2O), Ca-Fe arsenates, pharmacosiderite (KFe4 (AsO4)3(OH)4??6-7H2O), jarosite (K2Fe6(SO4)4 (OH)12) and arsenopyrite (FeAsS). Iron (III) oxyhydroxides contain variable levels of As from trace to about 22 wt% and Ca up to approximately 9 wt%. Finely ground ore and tailings samples were examined by bulk XAFS and selected mineral grains were analyzed by microfocused XAFS (micro-EXAFS) spectroscopy to reconcile the ambiguities of multiple As sources in the complex bulk EXAFS spectra. XANES spectra indicated that As occurs as As5+in all the samples. Micro-EXAFS spectra of individual iron (III) oxyhydroxide grains with varying As concentrations point to inner-sphere bidentate-binuclear arsenate complexes as the predominant form of As. There are indications for the presence of a second Fe shell corresponding to bidentate-mononuclear arrangement. Iron (III) oxyhydroxides with high As concentrations corresponding to maximum adsorption densities probably occur as nanoparticles. The discovery of Ca atoms around As in iron (III) oxyhydroxides at interatomic distances of 4.14-4.17 A?? and the coordination numbers suggest the formation of arseniosiderite-like nanoclusters by coprecipitation rather than simple adsorption of Ca onto iron (III) oxyhydroxides. Correlation of Ca with As in iron (III) oxyhydroxides as determined by electron microprobe analysis supports the coprecipitate origin for the presence of Ca in iron (III) oxyhydroxides. The samples containing higher abundances of ferric arsenates released higher As concentrations during the cyanidation tests. The presence of highly soluble ferric arsenates and Ca-Fe arsenates, and relatively unstable iron (III) oxyhydroxides with Fe/As molar ratios of less than 4 in the ore and process tailings suggests that not only the tailings in the impoundment will continue to release As, but also there is the potential for mobilization of As from the natural sources such as the unmined ore. ?? 2004 Elsevier Ltd.

  14. Speciation and characterization of arsenic in gold ores and cyanidation tailings using X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Paktunc, Dogan; Foster, Andrea; Heald, Steve; Laflamme, Gilles

    2004-03-01

    The knowledge of mineralogy and molecular structure of As is needed to better understand the stability of As in wastes resulting from processing of gold ores. In this study, optical microscopy, scanning electron microscopy, electron microprobe, X-ray diffraction and X-ray absorption fine structure (XAFS) spectroscopy (including both XANES and EXAFS regimes) were employed to determine the mineralogical composition and local coordination environment of As in gold ores and process tailings from bench-scale tests designed to mimic a common plant practice. Arsenic-bearing minerals identified in the ores and tailings include iron (III) oxyhydroxides, scorodite (FeAsO 4·2H 2O), ferric arsenates, arseniosiderite (Ca 2Fe 3(AsO 4) 3O 2·3H 2O), Ca-Fe arsenates, pharmacosiderite (KFe 4(AsO 4) 3(OH) 4·6-7H 2O), jarosite (K 2Fe 6(SO 4) 4(OH) 12) and arsenopyrite (FeAsS). Iron (III) oxyhydroxides contain variable levels of As from trace to about 22 wt% and Ca up to approximately 9 wt%. Finely ground ore and tailings samples were examined by bulk XAFS and selected mineral grains were analyzed by microfocused XAFS (micro-EXAFS) spectroscopy to reconcile the ambiguities of multiple As sources in the complex bulk EXAFS spectra. XANES spectra indicated that As occurs as As 5+in all the samples. Micro-EXAFS spectra of individual iron (III) oxyhydroxide grains with varying As concentrations point to inner-sphere bidentate-binuclear arsenate complexes as the predominant form of As. There are indications for the presence of a second Fe shell corresponding to bidentate-mononuclear arrangement. Iron (III) oxyhydroxides with high As concentrations corresponding to maximum adsorption densities probably occur as nanoparticles. The discovery of Ca atoms around As in iron (III) oxyhydroxides at interatomic distances of 4.14-4.17 Å and the coordination numbers suggest the formation of arseniosiderite-like nanoclusters by coprecipitation rather than simple adsorption of Ca onto iron (III) oxyhydroxides. Correlation of Ca with As in iron (III) oxyhydroxides as determined by electron microprobe analysis supports the coprecipitate origin for the presence of Ca in iron (III) oxyhydroxides. The samples containing higher abundances of ferric arsenates released higher As concentrations during the cyanidation tests. The presence of highly soluble ferric arsenates and Ca-Fe arsenates, and relatively unstable iron (III) oxyhydroxides with Fe/As molar ratios of less than 4 in the ore and process tailings suggests that not only the tailings in the impoundment will continue to release As, but also there is the potential for mobilization of As from the natural sources such as the unmined ore.

  15. Temperature micro-mapping and redox conditions of a chlorite zoning pattern in green-schist facies fault zone

    NASA Astrophysics Data System (ADS)

    Trincal, Vincent; Lanari, Pierre; Lacroix, Brice; Buatier, Martine D.; Charpentier, Delphine; Labaume, Pierre; Muñoz, Manuel

    2014-05-01

    Faults are major discontinuities driving fluid flows and playing a major role in precipitation of ore deposits. Mineral paragenesis and crystal chemistry depend on Temperature (T) condition, fluid composition but also on the redox environment of precipitation. The studied samples come from the Pic de Port Vieux thrust sheet, a minor thrust sheet associated to Gavarnie thrust fault zone (Central Pyrenees). The Pic de Port Vieux Thrust sheet comprises a 1-20 meter thick layer of Triassic red beds and mylonitized Cretaceous limestone. The thrust sheet is affected by faults and cleavage; the other important deformation product is a set of veins filled by quartz and chlorite. Microstructural and mineralogical investigations were performed based on the previous work of Grant (1992). The crystallization of chlorite is syn-tectonic and strongly controlled by the fluid circulation during the Gavarnie thrust sheet emplacement. Chlorite precipitated in extension veins, crack-seal shear veins or in open cavities. The chlorite filling the open cavities occurs as pseudo-uniaxial plates arranged in rosette-shaped aggregates. These aggregates appear to have developed as a result of radial growth of the chlorite platelets. According to point and microprobe X-ray images, these chlorites display oscillatory chemical zoning patterns with alternating iron rich and magnesium rich bands. The chlorite composition ranges from Fe rich pole (Si2.62Al1.38O10(Al1.47Fe1.87Mg2.61)6(OH)8) to Mg rich pole (Si2.68Al1.31O10(Al1.45Fe1.41Mg3.06)6(OH)8). In metamorphic rocks, zoning pattern or rimmed minerals results for varying P or T conditions and can be used to unravel the P-T history of the sample. In the present study, temperature maps are derived from standardized microprobe X-ray images using the program XMapTools (Lanari et al 2014). The (Fe3+/Fetot) value in chlorite was directly measured using μXANES spot analyses collected at the Fe-K edge. The results indicate a homogeneous temperature of 300-350° C throughout the crystallization. This result excludes the T as the main parameter to explain the Fe and Mg zoning patterns. Several other origins can be proposed and discussed in order to understand zoning patterns such as fluid chemistry, pressure, pH or redox variations of the fluid. Grant, N.T., 1992. Post-emplacement extension within a thrust sheet from the central Pyrenees. Journal of the Geological Society 149, 775-792. Lanari, P., Vidal, O., De Andrade, V., Dubacq, B., Lewin, E., Grosch, E.G., Schwartz, S., 2014. XMapTools: A MATLAB©-based program for electron microprobe X-ray image processing and geothermobarometry. Computers & Geosciences 62, 227-240.

  16. Foliar manganese accumulation by Maytenus founieri (Celastraceae) in its native New Caledonian habitats: populational variation and localization by X-ray microanalysis.

    PubMed

    Fernando, D R; Woodrow, I E; Jaffré, T; Dumontet, V; Marshall, A T; Baker, A J M

    2008-01-01

    Hyperaccumulation by plants is a rare phenomenon that has potential practical benefits. The majority of manganese (Mn) hyperaccumulators discovered to date occur in New Caledonia, and little is known about their ecophysiology. This study reports on natural populations of one such species, the endemic shrub Maytenus founieri. Mean foliar Mn concentrations of two populations growing on ultramafic substrates with varying soil pHs were obtained. Leaf anatomies were examined by light microscopy, while the spatial distributions of foliar Mn in both populations were examined by qualitative scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS). Plants growing on two different substrates were found to have very different mean dry weight (DW) foliar Mn concentrations. Light microscopy showed that the leaves had very distinct thick dermal structures, consisting of multiple layers of large cells in the hypodermis. In vivo X-ray microprobe analyses revealed that, in both populations, Mn sequestration occurred primarily in these dermal tissues. The finding here that foliar Mn is most highly localized in the nonphotosynthetic tissues of M. founieri contrasts with results from similar studies on other woody species that accumulate high Mn concentrations in their shoots.

  17. Ottensite, brizziite and mopungite from Pereta mine (Tuscany, Italy): new occurrences and crystal structure refinement of mopungite

    NASA Astrophysics Data System (ADS)

    Bittarello, Erica; Cámara, Fernando; Ciriotti, Marco E.; Marengo, Alessandra

    2015-08-01

    Ottensite, Na3 (Sb2O3)(SbS3)·3H2O, brizziite, NaSbO3, and mopungite, NaSb(OH)6, have been found on several specimens from the antimony mine of Pereta (Grosseto, Tuscany, Italy). Ottensite from Pereta mine occurs as brilliant reddish-brown spheroidal aggregates, with a diameter up to 0.2 mm, formed by radially oriented individuals. These aggregates are associated with well-shaped tabular and pseudocubic colourless crystals of mopungite and platy aggregates of brizziite. This is the second world occurrence of ottensite and brizziite. The mineral species were characterized by electron microprobe analysis, X-ray diffraction study and microRaman spectroscopy. Single-crystal X-ray diffraction data were collected on a twinned crystal of mopungite and the structure was for the first time refined on a natural sample in space group P42/ n [unit cell parameters a = 8.036(3) Å, c = 7.926(6) Å, V = 511.88(5) Å3, Z = 4] obtaining an R 1 -index of 5.17, wR 2 of 13.52 and GooF of 1.247.

  18. Zirconium, hafnium, and rare earth element partition coefficients for ilmenite and other minerals in high-Ti lunar mare basalts - An experimental study

    NASA Technical Reports Server (NTRS)

    Mckay, G.; Wagstaff, J.; Yang, S.-R.

    1986-01-01

    Partition coefficients were determined for Gd, Lu, Hf and Zr among ilmenite, armalcolite, and synthetic high-Ti mare basaltic melts at temperatures from 1122 deg to 1150 deg, and at oxygen fugacities of IW x 10 exp 0.5, by in situ analysis with an electron microprobe, using samples doped to present concentration levels. Coefficients for Zr were also measured for samples containing 600-1600 ppm Zr using this microprobe. In addition, coefficients were determined for Hf and Zr between chromian ulvospinel and melt, for Hf between pigeonite and melt, and for Lu between olivine and melt by microprobe analysis of samples doped to present levels. Values measured using the microprobe were in agreement with the values measured by analyzing mineral separates from the same run products by isotope dilution. Coefficient values for ilmenite are less than 0.01 for the LREE, are around 0.1 for the HREE, and are several times greater than this for Zr and Hf.

  19. Time-resolved X-ray diffraction microprobe studies of the conversion of cellulose I to ethylenediamine-cellulose I

    PubMed Central

    Nishiyama, Yoshiharu; Wada, Masahisa; Hanson, B. Leif

    2012-01-01

    Structural changes during the treatment of films of highly crystalline microfibers of Cladophora cellulose with ethylenediamine (EDA) have been studied by time-resolved X-ray microprobe diffraction methods. As EDA penetrates the sample and converts cellulose I to EDA-cellulose I, the measured profile widths of reflections reveal changes in the shapes and average dimensions of cellulose I and EDA-cellulose I crystals. The (200) direction of cellulose I is most resistant to EDA penetration, with EDA penetrating most effectively at the hydrophilic edges of the hydrogen bonded sheets of cellulose chains. Most of the cellulose chains in the initial crystals of cellulose I are incorporated into crystals of EDA-cellulose I. The size of the emerging EDA-cellulose I crystals is limited to about half of their size in cellulose I, most likely due to strains introduced by the penetration of EDA molecules. There is no evidence of any gradual structural transition from cellulose I to EDA-cellulose I involving a continuously changing intermediate phase. Rather, the results point to a rapid transition to EDA-cellulose I in regions of the microfibrils that have been penetrated by EDA. PMID:22693365

  20. Long-term clinical evaluation of endodontically treated teeth by 15 F CO2 laser microprobe: three years clinical follow-up of 1512 root canals--in-vivo study

    NASA Astrophysics Data System (ADS)

    Kesler, Gavriel; Koren, Rumelia; Kesler, Anat; Hay, Nissim; Gal, Rivka

    1999-05-01

    The purpose of this study was to determine the efficiency of 15 F CO2 laser microprobe, in cases of periapical lesions, by eliminating the pathological reaction caused by certain species of bacteria, reduction of reinfection and stimulation of osteogenesis in the periapical region. Until now, no suitable delivery fiber existed for CO2 laser endodontic radiation in the apical region where it is most difficult to eliminate the pulp tissue using conventional methods. To overcome this problem, Sharplan laser designed a microprobe that reaches closer to the apex, distributing the energy density to a smaller area of the root canal, thus favorably increasing the thermal effects. The study was conducted on 900 teeth, divided in two groups. 468 were new case, carefully selected according to strict parameters such as: wide periapical translucency over 1mm, supported by digital x-ray, with a lesion of 3mm and more. All root canals were mechanically prepared in the conventional method up to size 35, Physiological saline solution served as finding solution and were treated by 15 F CO2 laser microprobe for 60 pulses repeatedly. The temperature at the surrounding tissue of the root did not exceed 38 degrees C filling of the canal was possible at the same appointment, without antibiotical treatment. 432 of the cases, which were referred to us by other dentists, after an unsuccessful treatment according to the classical therapy, were treated by the same laser therapy. Follow up was performed by clinical examination, and digital x-ray taken, during and after treatment as well as after 3, 6, 9, 12 month. The result demonstrate 98% success rate in both study groups, according to objective criteria for a successful treatment such as: reduction of apical translucency after 2- 6 months, freedom form clinical complains, and no need for periapical surgery.

  1. Using refractive optics to broaden the focus of an X-ray mirror.

    PubMed

    Laundy, David; Sawhney, Kawal; Dhamgaye, Vishal

    2017-07-01

    X-ray mirrors are widely used at synchrotron radiation sources for focusing X-rays into focal spots of size less than 1 µm. The ability of the beamline optics to change the size of this spot over a range up to tens of micrometres can be an advantage for many experiments such as X-ray microprobe and X-ray diffraction from micrometre-scale crystals. It is a requirement that the beam size change should be reproducible and it is often essential that the change should be rapid, for example taking less than 1 s, in order to allow high data collection rates at modern X-ray sources. In order to provide a controlled broadening of the focused spot of an X-ray mirror, a series of refractive optical elements have been fabricated and installed immediately before the mirror. By translation, a new refractive element is moved into the X-ray beam allowing a variation in the size of the focal spot in the focusing direction. Measurements using a set of prefabricated refractive structures with a test mirror showed that the focused beam size could be varied from less than 1 µm to over 10 µm for X-rays in the energy range 10-20 keV. As the optics is in-line with the X-ray beam, there is no effect on the centroid position of the focus. Accurate positioning of the refractive optics ensures reproducibility in the focused beam profile and no additional re-alignment of the optics is required.

  2. Using refractive optics to broaden the focus of an X-ray mirror

    PubMed Central

    Dhamgaye, Vishal

    2017-01-01

    X-ray mirrors are widely used at synchrotron radiation sources for focusing X-rays into focal spots of size less than 1 µm. The ability of the beamline optics to change the size of this spot over a range up to tens of micrometres can be an advantage for many experiments such as X-ray microprobe and X-ray diffraction from micrometre-scale crystals. It is a requirement that the beam size change should be reproducible and it is often essential that the change should be rapid, for example taking less than 1 s, in order to allow high data collection rates at modern X-ray sources. In order to provide a controlled broadening of the focused spot of an X-ray mirror, a series of refractive optical elements have been fabricated and installed immediately before the mirror. By translation, a new refractive element is moved into the X-ray beam allowing a variation in the size of the focal spot in the focusing direction. Measurements using a set of prefabricated refractive structures with a test mirror showed that the focused beam size could be varied from less than 1 µm to over 10 µm for X-rays in the energy range 10–20 keV. As the optics is in-line with the X-ray beam, there is no effect on the centroid position of the focus. Accurate positioning of the refractive optics ensures reproducibility in the focused beam profile and no additional re-alignment of the optics is required. PMID:28664880

  3. On the distribution of uranium in hair: Non-destructive analysis using synchrotron radiation induced X-ray fluorescence microprobe techniques

    NASA Astrophysics Data System (ADS)

    Israelsson, A.; Eriksson, M.; Pettersson, H. B. L.

    2015-06-01

    In the present study the distribution of uranium in single human hair shafts has been evaluated using two synchrotron radiation (SR) based micro X-ray fluorescence techniques; SR μ-XRF and confocal SR μ-XRF. The hair shafts originated from persons that have been exposed to elevated uranium concentrations. Two different groups have been studied, i) workers at a nuclear fuel fabrication factory, exposed mainly by inhalation and ii) owners of drilled bedrock wells exposed by ingestion of water. The measurements were carried out on the FLUO beamline at the synchrotron radiation facility ANKA, Karlsruhe. The experiment was optimized to detect U with a beam size of 6.8 μm × 3 μm beam focus allowing detection down to ppb levels of U in 10 s (SR μ-XRF setup) and 70 s (SR confocal μ-XRF setup) measurements. It was found that the uranium was present in a 10-15 μm peripheral layer of the hair shafts for both groups studied. Furthermore, potential external hair contamination was studied by scanning of unwashed hair shafts from the workers. Sites of very high uranium signal were identified as particles containing uranium. Such particles, were also seen in complementary analyses using variable pressure electron microscope coupled with energy dispersive X-ray analyzer (ESEM-EDX). However, the particles were not visible in washed hair shafts. These findings can further increase the understanding of uranium excretion in hair and its potential use as a biomonitor.

  4. Quantitative X-ray Map Analyser (Q-XRMA): A new GIS-based statistical approach to Mineral Image Analysis

    NASA Astrophysics Data System (ADS)

    Ortolano, Gaetano; Visalli, Roberto; Godard, Gaston; Cirrincione, Rosolino

    2018-06-01

    We present a new ArcGIS®-based tool developed in the Python programming language for calibrating EDS/WDS X-ray element maps, with the aim of acquiring quantitative information of petrological interest. The calibration procedure is based on a multiple linear regression technique that takes into account interdependence among elements and is constrained by the stoichiometry of minerals. The procedure requires an appropriate number of spot analyses for use as internal standards and provides several test indexes for a rapid check of calibration accuracy. The code is based on an earlier image-processing tool designed primarily for classifying minerals in X-ray element maps; the original Python code has now been enhanced to yield calibrated maps of mineral end-members or the chemical parameters of each classified mineral. The semi-automated procedure can be used to extract a dataset that is automatically stored within queryable tables. As a case study, the software was applied to an amphibolite-facies garnet-bearing micaschist. The calibrated images obtained for both anhydrous (i.e., garnet and plagioclase) and hydrous (i.e., biotite) phases show a good fit with corresponding electron microprobe analyses. This new GIS-based tool package can thus find useful application in petrology and materials science research. Moreover, the huge quantity of data extracted opens new opportunities for the development of a thin-section microchemical database that, using a GIS platform, can be linked with other major global geoscience databases.

  5. Strategies for Analyzing Sub-Micrometer Features with the FE-EPMA

    NASA Astrophysics Data System (ADS)

    McSwiggen, P.; Armstrong, J. T.; Nielsen, C.

    2013-12-01

    Changes in column design and electronics, as well as new types of spectrometers and analyzing crystals, have significantly advanced electron microprobes, in terms of stability, reproducibility and detection limits. A major advance in spatial resolution has occurred through the use of the field emission electron gun. The spatial resolution of an analysis is controlled by the diameter of the electron beam and the amount of scatter that takes place within the sample. The beam diameter is controlled by the column and type of electron gun being used. The accelerating voltage and the average atomic number/density of the sample control the amount of electron scatter within the sample. However a large electron interaction volume does not necessarily mean a large analytical volume. The beam electrons may spread out within a large volume, but if the electrons lack sufficient energy to produce the X-ray of interest, the analytical volume could be significantly smaller. Therefore there are two competing strategies for creating the smallest analytical volumes. The first strategy is to reduce the accelerating voltage to produce the smallest electron interaction volume. This low kV analytical approach is ultimately limited by the size of the electron beam itself. With a field emission gun, normally the smallest analytical area is achieved at around 5-7 kV. At lower accelerating voltages, the increase in the beam diameter begins to overshadow the reduction in internal scattering. For tungsten filament guns, the smallest analytical volume is reached at higher accelerating voltages. The second strategy is to minimize the overvoltage during the analysis. If the accelerating voltage is only 1-3 kV greater than the critical ionization energy for the X-ray line of interest, then even if the overall electron interaction volume is large, those electrons quickly loose sufficient energy to produce the desired X-rays. The portion of the interaction volume in which the desired X-rays will be produce will be very small and very near the surface. Both strategies have advantages and disadvantages depending on the ultimate goal of the analysis and the elements involved. This work will examine a number of considerations when attempting to decide which approach is best for a given analytical situation. These include: (1) the size of the analytical volumes, (2) minimum detection limits, (3) quality of the matrix corrections, (4) secondary fluorescence, (5) effects of surface contamination, oxide layers, and carbon coatings. This work is based on results largely from the Fe-Ni binary. A simple conclusion cannot be draw as to which strategy is better overall. The determination is highly system dependent. For many mineral systems, both strategies used in combination will produce the best results. Using multiple accelerating voltages to preform a single analysis allows the analyst to optimize their analytical conditions for each element individually.

  6. Reverse engineering the ancient ceramic technology based on X-ray fluorescence spectromicroscopy

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

    Sciau, Philippe; Leon, Yoanna; Goudeau, Philippe

    2011-07-06

    We present results of X-ray fluorescence (XRF) microprobe analyses of ancient ceramic cross-sections aiming at deciphering the different firing protocols used for their production. Micro-focused XRF elemental mapping, Fe chemical mapping and Fe K-edge X-ray absorption near edge structure spectroscopy were performed on pre-sigillata ceramics from southern Gaul, and terra Sigillata vessels from Italy and southern Gaul. Pieces from the different workshops and regions showed significant difference in the starting clay material, clay conditioning and kiln firing condition. By contrast, sherds from the same workshop exhibited more subtle differences and possible misfirings. Understanding the precise firing conditions and protocols wouldmore » allow recreation of kilns for various productions. Furthermore, evolution and modification of kiln design would shed some light on how ancient potters devised solutions to diverse technological problems they encountered.« less

  7. Concrete alteration due to 55 years of exposure to river water: Chemical and mineralogical characterisation

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

    Rosenqvist, Martin; Bertron, Alexandra; Fridh, Katja

    This article presents a study on concrete alteration mechanisms due to 55 years of exposure to river water. Many hydro power structures in cold regions suffer from concrete deterioration at the waterline. Progressive disintegration of the concrete surface leads to exposure of the coarse aggregate and eventually the reinforcing steel. Concrete cylinders drilled out at four vertically different locations on the upstream face of a concrete dam were analysed by electron microprobe analysis, X-ray diffraction, thermogravimetry and scanning electron microscopy. Long-term exposure to the river water, which is regarded as soft water, has led to chemical and mineralogical zonation ofmore » the cement paste. Up to five zones with different chemical and mineralogical composition, parallel to the upstream face, were observed in the outermost 8–9 mm of the concrete. Decalcification, precipitation of secondary ettringite and the formation of a magnesium-rich silica gel constitute the major changes that define the zones.« less

  8. Reverse engineering the physical chemistry of making Egyptian faience through compositional analysis of the cementation process

    NASA Astrophysics Data System (ADS)

    Pourattar, Parisa

    The cementation process of making Egyptian faience, reported by Hans Wulff from a workshop in Qom, Iran, has not been easy to replicate and various views have been set forth to understand the transport of materials from the glazing powder to the surfaces of the crushed quartz beads. Replications of the process fired to 950° C and under-fired to 850° C were characterized by electron beam microprobe analysis (EPMA), petrographic thin section analysis, and scanning electron microscopy with energy dispersive x-ray analysis (SEM-EDS). Chemical variations were modeled using thermal data, phase diagrams, and copper vaporization experiments. These replications were compared to 52 examples from various collections, including 20th century ethnographic collections of beads, glazing powder and plant ash, 12th century CE beads and glazing powder from Fustat (Old Cairo), Egypt, and to an earlier example from Abydos, Egypt in the New Kingdom and to an ash example from the Smithsonian Institution National Museum of Natural History.

  9. Heat pipe fatigue test specimen: Metallurgical evaluation

    NASA Technical Reports Server (NTRS)

    Walak, Steven E.; Cronin, Michael J.; Grobstein, Toni

    1992-01-01

    An innovative creep/fatigue test was run to simulate the temperature, mechanical load, and sodium corrosion conditions expected in a heat pipe designed to supply thermal energy to a Stirling cycle power converter. A sodium-charged Inconel 718 heat pipe with a Nickel 200 screen wick was operated for 1090 hr at temperatures between 950 K (1250 F) and 1050 K (1430 F) while being subjected to creep and fatigue loads in a servo-hydraulic testing machine. After testing, the heat pipe was sectioned and examined using optical microscopy, scanning electron microscopy, and electron microprobe analysis with wavelength dispersive x-ray spectroscopy. The analysis concentrated on evaluating topographic, microstructural, and chemical changes in the sodium exposed surfaces of the heat pipe wall and wick. Surface changes in the evaporator, condenser, and adiabatic sections of the heat pipe were examined in an effort to correlate the changes with the expected sodium environment in the heat pipe. This report describes the setup, operating conditions, and analytical results of the sodium heat pipe fatigue test.

  10. Analysis of ablation debris from natural and artificial iron meteorites

    NASA Technical Reports Server (NTRS)

    Blanchard, M. B.; Davis, A. S.

    1977-01-01

    Artificial ablation studies were performed on iron and nickel-iron samples using an arc-heated plasma of ionized air. Experiment conditions simulated a meteoroid traveling about 12 km/sec at an altitude of 70 km. The artificially produced fusion crusts and ablation debris show features very similar to natural fusion crusts of the iron meteorites Boguslavka, Norfork, and N'Kandhla and to magnetic spherules recovered from Mn nodules. X-ray diffraction, electron microprobe, optical, and scanning electron microscope analyses reveal that important mineralogical, elemental, and textural changes occur during ablation. Some metal is melted and ablated. The outer margin of the melted rind is oxidized and recrystallizes as a discontinuous crust of magnetite and wustite. Adjacent to the oxidized metallic ablation zone is an unoxidized metallic ablation zone in which structures such as Widmannstatten bands are obliterated as the metal is transformed to unequilibrated alpha 2 nickel-iron. Volatile elements are vaporized and less volatile elements undergo fractionation.

  11. Filling the holes in the CaFe4As3 structure: Synthesis and magnetism of CaCo5As3

    NASA Astrophysics Data System (ADS)

    Rosa, P. F. S.; Scott, B. L.; Ronning, F.; Bauer, E. D.; Thompson, J. D.

    2017-07-01

    Here, we investigate single crystals of CaCo5As3 by means of single-crystal x-ray diffraction, microprobe, magnetic susceptibility, heat capacity, and pressure-dependent transport measurements. CaCo5As3 shares the same structure of CaFe4As3 with an additional Co atom filling a lattice vacancy and undergoes a magnetic transition at TM=16 K associated with a frustrated magnetic order. CaCo5As3 displays metallic behavior and its Sommerfeld coefficient (γ =70 mJ/mol K2) indicates a moderate enhancement of electron-electron correlations. Transport data under pressures to 2.5 GPa reveal a suppression of TM at a rate of -0.008 K/GPa. First-principles electronic structure calculations show a complex three-dimensional band structure and magnetic moments that depend on the local environment at each Co site. Our results are compared with previous data on CaFe4As3 and provide a scenario for a magnetically frustrated ground state in this family of compounds.

  12. The composition of coexisting jarosite-group minerals and water from the Richmond mine, Iron Mountain, California

    USGS Publications Warehouse

    Jamieson, Heather E.; Robinson, Clare; Alpers, Charles N.; Nordstrom, D. Kirk; Poustovetov, Alexei; Lowers, Heather A.

    2005-01-01

    Jarosite-group minerals accumulate in the form of stalactites and fine-grained mud on massive pyrite in the D drift of the Richmond mine, Iron Mountain, California. Water samples were collected by placing beakers under the dripping stalactites and by extracting pore water from the mud using a centrifuge. The water is rich in Fe3+ and SO4 2−, with a pH of approximately 2.1, which is significantly higher than the extremely acidic waters found elsewhere in the mine. Electron-microprobe analysis and X-ray mapping indicate that the small crystals (<10 μm in diameter) are compositionally zoned with respect to Na and K, and include hydronium jarosite corresponding to the formula (H3O)0.6K0.3Na0.1Fe3 3+(SO4)2(OH)6. The proton-microprobe analyses indicate that the jarosite-group minerals contain significant amounts of As, Pb and Zn, and minor levels of Bi, Rb, Sb, Se, Sn and Sr. Speciation modeling indicates that the drip waters are supersaturated with respect to jarosite-group minerals. The expected range in composition of jarosite-group solid-solution in equilibrium with the pore water extracted from the mud was found to be consistent with the observed range in composition.

  13. Thermodynamics and kinetics of the sulfation of porous calcium silicate

    NASA Technical Reports Server (NTRS)

    Miller, R. A.; Kohl, F. J.

    1981-01-01

    The sulfation of plasma sprayed calcium silicate in flowing SO2/air mixtures at 900 and 1000 C was investigated thermogravimetrically. Reaction products were analyzed using electron microprobe and X-ray diffraction analysis techniques, and results were compared with thermodynamic predictions. The percentage, by volume, of SO2 in air was varied between 0.036 and 10 percent. At 10 percent SO2 the weight gain curve displays a concave downward shoulder early in the sulfation process. An analytical model was developed which treats the initial process as one which decays exponentially with increasing time and the subsequent process as one which decays exponentially with increasing weight gain. At lower SO2 levels the initial rate is controlled by the reactant flow rate. At 1100 C and 0.036 percent SO2 there is no reaction, in agreement with thermodynamic predictions.

  14. AS SPECIATION AND EFFECTS OF PH AND PHOSPHATE ON THE MOBILIZATION OF AS IN SOILS FROM A LEAD SMELTING SITE. PUBLISHED IN ADVANCED PHOTON SOURCE ACTIVITY REPORT 2003.

    EPA Science Inventory

    Arsenic in soils from the Asarco lead smelter in East Helena, Montana was characterized by X-ray absorption spectroscopy (XAS). Arsenic oxidation state and mineralogy were analyzed as a function of depth and surface distribution using bulk and microprobe XAS. These results were c...

  15. Application of Synchrotron Microprobe Methods to Solid-Phase Speciation of Metals and Metalloids in House Dust

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

    S Walker; H Jamieson; P Rasmussen

    2011-12-31

    Determination of the source and form of metals in house dust is important to those working to understand human and particularly childhood exposure to metals in residential environments. We report the development of a synchrotron microprobe technique for characterization of multiple metal hosts in house dust. We have applied X-ray fluorescence for chemical characterization and X-ray diffraction for crystal structure identification using microfocused synchrotron X-rays at a less than 10 {micro}m spot size. The technique has been evaluated by application to archived house dust samples containing elevated concentrations of Pb, Zn, and Ba in bedroom dust, and Pb and Asmore » in living room dust. The technique was also applied to a sample of soil from the corresponding garden to identify linkages between indoor and outdoor sources of metals. Paint pigments including white lead (hydrocerussite) and lithopone (wurtzite and barite) are the primary source of Pb, Zn, and Ba in bedroom dust, probably related to renovation activity in the home at the time of sampling. The much lower Pb content in the living room dust shows a relationship to the exterior soil and no specific evidence of Pb and Zn from the bedroom paint pigments. The technique was also successful at confirming the presence of chromated copper arsenate treated wood as a source of As in the living room dust. The results of the study have confirmed the utility of this approach in identifying specific metal forms within the dust.« less

  16. Measurements of the quantitative lateral analytical resolution at evaporated aluminium and silver layers with the JEOL JXA-8530F FEG-EPMA

    NASA Astrophysics Data System (ADS)

    Berger, D.; Nissen, J.

    2018-01-01

    The studies in this paper are part of systematic investigations of the lateral analytical resolution of the field emission electron microprobe JEOL JXA-8530F. Hereby, the quantitative lateral resolution, which is achieved in practise, is in the focus of interest. The approach is to determine the minimum thickness of a metallic layer for which an accurate quantitative element analysis in cross-section is still possible. Previous measurements were accomplished at sputtered gold (Z = 79) layers, where a lateral resolution in the range of 140 to 170 nm was achieved at suitable parameters of the microprobe. To study the Z-dependence of the lateral resolution, now aluminium (Z = 13) resp. silver (Z = 47) layers with different thicknesses were generated by evaporation and prepared in cross-section subsequently by use of a focussed Ga-ion beam (FIB). Each layer was analysed quantitatively with different electron energies. The thinnest layer which can be resolved specifies the best lateral resolution. These measured values were compared on the one hand with Monte Carlo simulations and on the other hand with predictions from formulas from the literature. The measurements fit well to the simulated and calculated values, except the ones at the lowest primary electron energies with an overvoltage below ˜ 2. The reason for this discrepancy is not clear yet and has to be clarified by further investigations. The results apply for any microanalyser - even with energy-dispersive X-ray spectrometry (EDS) detection - if the probe diameters, which might deviate from those of the JEOL JXA-8530F, at suitable analysing parameters are considered.

  17. Compact x-ray source and panel

    DOEpatents

    Sampayon, Stephen E [Manteca, CA

    2008-02-12

    A compact, self-contained x-ray source, and a compact x-ray source panel having a plurality of such x-ray sources arranged in a preferably broad-area pixelized array. Each x-ray source includes an electron source for producing an electron beam, an x-ray conversion target, and a multilayer insulator separating the electron source and the x-ray conversion target from each other. The multi-layer insulator preferably has a cylindrical configuration with a plurality of alternating insulator and conductor layers surrounding an acceleration channel leading from the electron source to the x-ray conversion target. A power source is connected to each x-ray source of the array to produce an accelerating gradient between the electron source and x-ray conversion target in any one or more of the x-ray sources independent of other x-ray sources in the array, so as to accelerate an electron beam towards the x-ray conversion target. The multilayer insulator enables relatively short separation distances between the electron source and the x-ray conversion target so that a thin panel is possible for compactness. This is due to the ability of the plurality of alternating insulator and conductor layers of the multilayer insulators to resist surface flashover when sufficiently high acceleration energies necessary for x-ray generation are supplied by the power source to the x-ray sources.

  18. Correlative Cryo-Tem Cryo-Stxm and Cryo-Shxm Investigation of Selenium Bioreduction in a Contaminated Aquifer

    NASA Astrophysics Data System (ADS)

    Fakra, S.; Luef, B.; Tyliszczak, T.; Castelle, C. J.; Mullin, S. W.; Hug, L. A.; Williams, K. H.; Marcus, M.; Banfield, J. F.

    2015-12-01

    Accurate mapping of the composition and ultrastructure of minerals and cells is key to understanding biogeochemical process in contaminated environments. Here we developed two apparatus that allow correlation of cryogenic transmission electron microscopy (TEM), synchrotron hard X-ray microprobe (SHXM) and scanning transmission X-ray microscopy (STXM) datasets. These cryogenic methods enabled precise determination of the distribution, valence state and structure of selenium in intact biofilms sampled during a biostimulation experiment in a contaminated aquifer near Rifle, CO, USA. Results were replicated in the laboratory via anaerobic selenate-reducing enrichment cultures. 16S rRNA analyses of field-derived biofilm indicated the dominance of Betaproteobacteria from the Comamonadaceae family, and uncultivated members of the Simplicispira genus. The major product in field and culture-derived biofilms consists of ~25-300 nm red amorphous Se0 aggregates of colloidal nanoparticles. Correlative analyses of the cultures provided direct evidence for microbial dissimilatory reduction of Se(VI) to Se(IV) to Se0. X-ray diffraction and Se K-edge extended X-ray absorption fine structure spectroscopy revealed red amorphous Se0 with a first shell Se-Se interatomic distance of 2.339 ± 0.003 Å. STXM showed that these aggregates are strongly associated with a protein-rich biofilm matrix containing acidic polysaccharides. From Rifle groundwater, we isolated a strain that shares 98.9% 16S rRNA gene sequence identity with Dechloromonas aromatica RCB and grows anaerobically by oxidizing acetate and reducing selenate. We refer to this isolate as Dechloromonas selenatis strain RGW99. 3D cryo-electron tomography showed that Se0 particles do not form inside the cytoplasm but rather originate in the cell membrane. The end product of selenate reduction by D. selenatis is 240 ± 66 nm diameter red amorphous Se0 colloidal aggregates. This product was found to be stable for months. Overall, these results established a role for D. selenatis RGW99 in selenate reduction in the Rifle aquifer and provided new insights into the nature and stability of selenium bioreduction products in the subsurface.

  19. Femtosecond laser-electron x-ray source

    DOEpatents

    Hartemann, Frederic V.; Baldis, Hector A.; Barty, Chris P.; Gibson, David J.; Rupp, Bernhard

    2004-04-20

    A femtosecond laser-electron X-ray source. A high-brightness relativistic electron injector produces an electron beam pulse train. A system accelerates the electron beam pulse train. The femtosecond laser-electron X-ray source includes a high intra-cavity power, mode-locked laser and an x-ray optics system.

  20. Pore-scale characterization of biogeochemical controls on iron and uranium speciation under flow conditions.

    PubMed

    Pearce, Carolyn I; Wilkins, Michael J; Zhang, Changyong; Heald, Steve M; Fredrickson, Jim K; Zachara, John M

    2012-08-07

    Etched silicon microfluidic pore network models (micromodels) with controlled chemical and redox gradients, mineralogy, and microbiology under continuous flow conditions are used for the incremental development of complex microenvironments that simulate subsurface conditions. We demonstrate the colonization of micromodel pore spaces by an anaerobic Fe(III)-reducing bacterial species (Geobacter sulfurreducens) and the enzymatic reduction of a bioavailable Fe(III) phase within this environment. Using both X-ray microprobe and X-ray absorption spectroscopy, we investigate the combined effects of the precipitated Fe(III) phases and the microbial population on uranium biogeochemistry under flow conditions. Precipitated Fe(III) phases within the micromodel were most effectively reduced in the presence of an electron shuttle (AQDS), and Fe(II) ions adsorbed onto the precipitated mineral surface without inducing any structural change. In the absence of Fe(III), U(VI) was effectively reduced by the microbial population to insoluble U(IV), which was precipitated in discrete regions associated with biomass. In the presence of Fe(III) phases, however, both U(IV) and U(VI) could be detected associated with biomass, suggesting reoxidation of U(IV) by localized Fe(III) phases. These results demonstrate the importance of the spatial localization of biomass and redox active metals, and illustrate the key effects of pore-scale processes on contaminant fate and reactive transport.

  1. Application of X-ray photoelectron spectroscopy to the analysis of stainless-steel welding aerosols

    NASA Astrophysics Data System (ADS)

    Tandon, R. K.; Payling, R.; Chenhall, B. E.; Crisp, P. T.; Ellis, J.; Baker, R. S.

    1985-02-01

    Aerosol particles ("fume") from manual metal arc welding of stainless steel with E316L-16 electrodes were analysed by X-ray photoelectron spectroscopy. The inherent complexity of the particles required the use of a wide range of experimental techniques. These included IR spectrophotometry, TGA/DTA, XRF, XRD, AAS and electron microprobe analysis. The surface of the fume particles comprised ≈ 50 at% NaF and KF, ≈ 8 at.% soluble (probably K) chromate, ≈ 30 at% SiO 2 and several at.% transition-metal oxides, hydroxides or silicates. The fluorides and chromates were removed by washing to reveal a surface which was predominantly SiO 2 (≈ 60 at%) with the remainder comprising of transition-metal oxides, silicates and fluorides. Approximately 6 at% F remained on the surface of the water-washed particles, presumably as transition-metal fluoro-complexes. The water-soluble fraction of the fume contained K +, Na +, F - and CrO 2-4 ions in the mole ratio 5:5:4:3. When aerosol particles are deposited in lung tissues, water-soluble constituents would be expected to dissolve rapidly. In view of the suspected carcinogenicity of stainless steel welding fume, a bio-medical study of the combined effects of F - and CrO 2-4 ions on lung tissue is warranted.

  2. Atmospheric electron x-ray spectrometer

    NASA Technical Reports Server (NTRS)

    Feldman, Jason E. (Inventor); George, Thomas (Inventor); Wilcox, Jaroslava Z. (Inventor)

    2002-01-01

    The present invention comprises an apparatus for performing in-situ elemental analyses of surfaces. The invention comprises an atmospheric electron x-ray spectrometer with an electron column which generates, accelerates, and focuses electrons in a column which is isolated from ambient pressure by a:thin, electron transparent membrane. After passing through the membrane, the electrons impinge on the sample in atmosphere to generate characteristic x-rays. An x-ray detector, shaping amplifier, and multi-channel analyzer are used for x-ray detection and signal analysis. By comparing the resultant data to known x-ray spectral signatures, the elemental composition of the surface can be determined.

  3. Speciation of PM10 sources of airborne nonferrous metals within the 3-km zone of lead/zinc smelters.

    PubMed

    Batonneau, Yann; Bremard, Claude; Gengembre, Leon; Laureyns, Jacky; Le Maguer, Agnes; Le Maguer, Didier; Perdrix, Esperanza; Sobanska, Sophie

    2004-10-15

    The purpose of this study was to estimate the speciation of PM10 sources of airborne Pb, Zn, and Cd metals (PM10 is an aerosol standard of aerodynamic diameter less than 10 microm.) in the atmosphere of a 3 km zone surrounding lead/zinc facilities in operation for a century. Many powdered samples were collected in stacks of working units (grilling, furnace, and refinery), outdoor storages (ores, recycled materials), surrounding waste slag (4 Mt), and polluted topsoils (3 km). PM10 samples were generated from the raw powders by using artificial resuspension and collection devices. The bulk PM10 multielemental analyses were determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The proportions in mass of Pb (50%), Zn (40%), and Cd (1%) contents and associated metals (traces) reach the proportions of corresponding raw powdered samples of ores, recycled materials, and fumesize emissions of plants without specific enrichment. In contrast, Pb (8%) and Zn (15%) contents of PM10 of slag deposit were found to be markedly higher than those of raw dust, Pb (4%), and Zn (9%), respectively. In the same way, Pb (0.18%), Zn (0.20%), and Cd (0.004%) were enriched by 1.7, 2.1, and 2.3 times, respectively, in PM10 as compared with raw top-soil corresponding values. X-ray wavelength dispersive electron-microprobe (EM-WDS) microanalysis did not indicate well-defined phases or simple stoichiometries of all the PM10 samples atthe level of the spatial resolution (1 microm3). X-ray photoelectron spectroscopy (XPS) indicated that minor elements such as Cd, Hg, and C are more concentrated on the particle surface than in the bulk of PM10 generated by the smelting processes. (XPS) provided also the average speciation of the surface of PM10; Pb is mainly represented as PbSO4, Zn as ZnS, and Cd as CdS or CdSO4, and small amounts of coke were also detected. The speciation of bulk PM10 crystallized compounds was deduced from XRD diffractograms with a raw estimation of the relative quantities. PbS and ZnS were found to be the major phases in PM10 generated by the smelting facilities with PbSO4, PbSO4 x PbO, PbSO4 x 4PbO, Pb metal, and ZnO as minor phases. The slag waste PM10 was found to contain some amounts of PbCO3, PbSO4 x PbO, and ZnFe2O4 phases. The large heterogeneity at the level of the individual particle generates severe overlap of chemical information even at the microm scale using electron microprobe (WDS) and Raman microprobe techniques. Fortunately, scanning Raman microspectrometry combined with SIMPle-to-use Interactive Self-modeling Mixture Analysis (SIMPLISMA) performed the PM10 speciation at the level of individual particles. The speciation of major Pb, Zn, and Cd compounds of PM10 stack emissions and wind blown dust of ores and recycled materials were found to be PbSO4, PbSO4 x PbO, PbSO4 x 4PbO, PbO, metallic Pb, ZnS, ZnO, and CdS. The PM10 dust of slag waste was found to contain PbCO3, Pb(OH)2 x 2PbCO3, PbSO4 x PbO, and ZnS, while PM10-bound Pb, Zn of the top-soils contain Pb5(PO4)3Cl, ZnFe2O4 as well as Pb(II) and Zn(II) compounds adsorbed on Fe(III) oxides and in association with clays.

  4. 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.

  5. Ion microprobe, electron microprobe and cathodoluminescence data for Allende inclusions with emphasis on plagioclase chemistry

    NASA Technical Reports Server (NTRS)

    Hutcheon, I. D.; Steele, I. M.; Smith, J. V.; Clayton, R. N.

    1978-01-01

    Three Type B inclusions from the Allende meteorite have been analyzed. A grain-to-grain characterization of mineral chemistry and isotopic content was made possible by the use of a range of techniques, including luminescence and scanning electron microscopy and electron and ion microprobe analysis. Cathodoluminescence was used in fine-grained, optically opaque regions to distinguish between sub-micrometer phases, such as garnet and Si-rich material, subsequently identified by electron probe and scanning electron microscope analyses. Four types of luminescence patterns, due to twinning, primary sector zoning, alteration of boundaries and fractures, and shock effects, were identified in Allende plagioclase. Luminescence color exhibited a strong correlation with Mg content and provided a guide for an electron probe quantitative map of Mg and Na distributions. Ion microprobe studies of individual grains revealed large excesses of Mg-26.

  6. Mössbauer effect studies of Fe-C combinatorially sputtered thin films

    NASA Astrophysics Data System (ADS)

    Al-Maghrabi, M. A.; Sanderson, R. J.; Dunlap, R. A.

    2013-08-01

    Alloys of Fe1- x C x were produced using combinatorial sputtering methods. The composition of the films as a function of position was determined using electron microprobe techniques and the results have shown that a composition range of about 0.35 < x < 0.75 was obtained. X-ray diffraction methods were employed to study the structure of the thin films and showed that all portions of the films were amorphous or nanostructured. Room temperature 57Fe Mössbauer spectroscopy was utilized to study the atomic environment around the Fe atoms. Hyperfine field distributions of ferromagnetic alloys, as extracted from the Mössbauer analysis, suggested the existence of two classes of Fe sites: (1) classes of Fe sites that have primarily Fe neighbours corresponding to a high-field component in the distribution and (2) classes of Fe sites that have a greater number of C neighbours, corresponding to a low-field component. The magnetic splitting decreased as a function of increasing carbon concentration and alloys with x greater than about 0.68 were primarily paramagnetic in nature. These spectra exhibited distributions of quadrupole splitting with mean splitting in excess of 1.0 mm/s. This indicates a higher degree of local asymmetry around the Fe sites than typically seen in other Fe-metalloid systems.

  7. Fe-Mg substitution in aluminate spinels: effects on elastic properties investigated by Brillouin scattering

    NASA Astrophysics Data System (ADS)

    Bruschini, Enrico; Speziale, Sergio; Bosi, Ferdinando; Andreozzi, Giovanni B.

    2018-03-01

    We investigated by a multi-analytical approach (Brillouin scattering, X-ray diffraction and electron microprobe) the dependence of the elastic properties on the chemical composition of six spinels in the series (Mg1-x ,Fe x )Al2O4 (0 ≤ x ≤ 0.5). With the exception of C 12, all the elastic moduli (C 11, C 44, K S0 and G) are insensitive to chemical composition for low iron concentration, while they decrease linearly for higher Fe2+ content. Only C 12 shows a continuous linear increase with increasing Fe2+ across the whole compositional range under investigation. The high cation disorder showed by the sample with x = 0.202 has little or no influence on the elastic parameters. The range 0.202 < x < 0.388 bounds the percolation threshold (p c) for nearest neighbor interaction of Fe in the cation sublattices of the spinel structure. Below x = 0.202, the iron atoms are diluted in the system and far from each other, and the elastic moduli are nearly constant. Above x = 0.388, Fe atoms form extended interconnected clusters and show a cooperative behavior thus affecting the single-crystal elastic moduli. The elastic anisotropy largely increases with the introduction of Fe2+ in substitution of magnesium in spinel. This behavior is different with respect to other spinels containing transition metals such as Mn2+ and Co2+.

  8. Mach 1 oxidation of thoriated nickel chromium at 1204 C /2200 F/.

    NASA Technical Reports Server (NTRS)

    Lowell, C. E.; Sanders, W. A.

    1972-01-01

    Electropolished and ground samples of TD-NiCr were exposed to a 1-atm, Mach 1 gas stream at 1204 C for times up to 50 hr. The samples were subjected to both cyclic and isothermal exposure. Weight change, metal loss, X-ray diffraction, metallographic, and electron microprobe analyses were performed. Neither surface preparation nor cyclic-against-isothermal-exposure conditions had a strong effect on the oxidation behavior of the alloy. Initially, a Cr2O3 layer was formed whose volatilization resulted in a very rapid loss of metal - more than 40 microns in the first hour. At about 1 hr, the Cr2O3 layer broke down and NiO began to cover the surface. By 5 hr, the NiO had covered the surface and the rate of loss slowed. The rate-controlling step was diffusion of Cr through NiO.

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

    Connolly, J.R.

    Petrologic, bulk chemical, and mineralogic data are presented for 49 samples of tuffaceous rocks from core holes USW G-1 and UE-25a{number_sign}1 at Yucca Mountain, Nevada. Included, in descending stratigraphic order, are 11 samples from the Topopah Spring Member of the Paintbrush Tuff, 12 samples from the Tuffaceous Beds of Calico Hills, 3 samples from the Prow Pass Member of the Crater Flat Tuff, 20 samples from the Bullfrog Member of the Crater Flat Tuff and 3 samples from the Tram Member of the Crater Flat Tuff. The suite of samples contains a wide variety of petrologic types, including zeolitized, glassy,more » and devitrified tuffs. Data vary considerably between groups of samples, and include thin section descriptions (some with modal analyses for which uncertainties are estimated), electron microprobe analyses of mineral phases and matrix, mineral identifications by X-ray diffraction, and major element analyses with uncertainty estimates.« less

  10. Electron microprobe analysis of human labial gland secretory granules in cystic fibrosis

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

    Izutsu, K.; Johnson, D.; Schubert, M.

    1985-06-01

    X-ray microanalysis of freeze-dried labial gland cryosections revealed that Na concentration was doubled and the Ca/S concentration ratio was decreased in secretory granules of labial glands from patients with cystic fibrosis (CF) when compared with glands from normal subjects. Other results suggested that the decrease in the Ca/S concentration ratio resulted from an increase in S concentration. These findings imply that mucous granules in labial saliva showed a CF-related increase in Na and S content, and such changes would be expected to affect the rheology of the mucus after exocytosis. In contrast with a previous study in human parotid glands,more » no evidence was found for CF-related changes in cytoplasmic or nuclear Na, K, and Ca concentrations. Significant elemental differences were found between secretory granules and nuclei and cytoplasm of control cells.« less

  11. Development of nanosized lanthanum strontium aluminum manganite as electrodes for potentiometric oxygen sensor

    DOE PAGES

    Mullen, Max R.; Spirig, John V.; Hoy, Julia; ...

    2014-11-01

    Nanocrystalline La0.8Sr0.2Al0.9Mn0.1O3 (LSAM) was synthesized by a microwave-assisted citrate method, and characterized by electron microscopy and X-ray diffraction. Electrical behavior of LSAM was investigated by impedance spectroscopy and activation energy of conduction was obtained. Joining of sintered bodies of LSAM and yttria-stabilized tetragonal zirconia polycrystals (YTZP), an extensively studied oxygen ion conducting electrolyte, was examined by isostatic hot pressing methods. Characteristics of the joining region were evaluated with microprobe Raman spectroscopy, and products formed at the interface, primarily strontium zirconate, was confirmed by examination of high temperature chemical reaction between LSAM and YTZP powders. Finally, the electrical properties of themore » LSAM were exploited for development of a high temperature oxygen sensor in which LSAM functioned as the electrode and YTZP as electrolyte.« less

  12. Phase relations in the CuVS system

    USGS Publications Warehouse

    Wu, D.; Chang, L.L.Y.; Knowles, C.R.

    1986-01-01

    Phase relations in the system Cu-V-S were studied by using a sealedcapsule technique, reflected-light microscopy, X-ray powder diffraction and electron microprobe analysis. In the temperature range between 300 and 900 ??C, six vanadium sulfides exist in the V-S system. These are VS, V7S8, V3S4, V5S8, V3S5 and VS4. In the Cu-V-S system, three Cu-V sulfides are stable. Both Cu3VS4 (sulvanite) and CuV2S4 are cubic with a = 5.391 ?? 0.005 A ?? and a = 9.789 ?? 0.005 A ?? respectively, and the third has a composition Cu0.8V1.1S2. CuV2S4 forms equilibrium assemblages with all vanadium sulfides, which restricts their effects on the phase relations in the system to a small region. ?? 1986.

  13. The 1200 C cyclic oxidation behavior of two nickel-aluminum alloys (Ni3AL and NiAl) with additions of chromium, silicon, and titanium

    NASA Technical Reports Server (NTRS)

    Lowell, C. E.; Santoro, G. J.

    1972-01-01

    The alloys Ni3Al and NiAl with and without 1 and 3 atomic percent chromium, silicon, and titanium replacing the aluminum were cyclically oxidized at 1200 C for times to 200 hours, and the results were compared with those obtained with the alloy B-1900 subjected to the same oxidation process. The evaluation was based on metal recession, specific weight change, metallography, electron microprobe analysis, and X-ray diffraction. The oxidation resistance of Ni3Al was improved by Si, unaffected by Ti, and degraded by Cr. The oxidation resistance of NiAl was slightly improved by Ti, unaffected by Si, and degraded by Cr. The oxidation resistance of Ni3Al with 1 atomic percent Si was nearly equal to that of NiAl. Alloy B-1900 exhibited oxidation resistance comparable to that of Ni3Al + Cr compositions.

  14. Some wear studies on aircraft brake systems

    NASA Technical Reports Server (NTRS)

    Ho, T. L.

    1975-01-01

    An initial investigation of worn surfaces in friction pads and steel rotors used in current aircraft brakes was carried out using electron microprobe and X-ray diffraction analysis. It consists of the topographical study and the analysis of chemical element distribution. Based upon this initial examination, two approaches, microscopic and macroscopic have been conducted to interpret and formulate the wear mechanism of the aircraft brake materials. Microscopically, the wear particles were examined. The initiation and growth of surface cracks and the oxidation were emphasized in this investigation. Macroscopically, it has been found that, for the current copper based brake material sliding against 17-22 AS steel in a caliper brake, the surface temperature raised due to frictional heat is nonlinearly proportional to the load applied and slide time with speed at 1750 rpm. The wear of brake materials is then proportional to this temperature and is also a function of the melting temperature for copper.

  15. Trace Element Zoning and Incipient Metamictization in a Lunar Zircon: Application of Three Microprobe Techniques

    NASA Technical Reports Server (NTRS)

    Wopenka, Brigitte; Jollife, Bradley L.; Zinner, Ernst; Kremser, Daniel T.

    1996-01-01

    We have determined major (Si, Zr, Hf), minor (Al, Y, Fe, P), and trace element (Ca, Sc, Ti, Ba, REE, Th, U) concentrations and Raman spectra of a zoned, 200 microns zircon grain in lunar sample 14161,7069, a quartz monzodiorite breccia collected at the Apollo 14 site. Analyses were obtained on a thin section in situ with an ion microprobe, an electron microprobe, and a laser Raman microprobe. The zircon grain is optically zoned in birefringence, a reflection of variable (incomplete) metamictization resulting from zo- nation in U and Th concentrations. Variations in the concentrations of U and Th correlate strongly with those of other high-field-strength trace elements and with changes in Raman spectral parameters. Concentrations of U and Th range from 21 to 55 ppm and 6 to 31 ppm, respectively, and correlate with lower Raman peak intensities, wider Raman peaks, and shifted Si-O peak positions. Concentrations of heavy rare earth elements range over a factor of three to four and correlate with intensities of fluorescence peaks. Correlated variations in trace element concentrations reflect the original magmatic differentiation of the parental melt approx. 4 b.y. ago. Degradation of the zircon structure, as reflected by the observed Raman spectral parameters, has occurred in this sample over a range of alpha-decay event dose from approx. 5.2 x 10(exp 14) to 1.4 x 10(exp 15) decay events per milligram of zircon, as calculated from the U and Th concentrations. This dose is well below the approx. 10(exp 16) events per milligram cumulative dose that causes complete metamictization and indicates that laser Raman microprobe spectroscopy is an analytical technique that is very sensitive to the radiation-induced damage in zircon.

  16. The uniformity and imaging properties of some new ceramic scintillators

    NASA Astrophysics Data System (ADS)

    Chac, George T. L.; Miller, Brian W.; Shah, Kanai; Baldoni, Gary; Domanik, Kenneth J.; Bora, Vaibhav; Cherepy, Nerine J.; Seeley, Zachary; Barber, H. Bradford

    2012-10-01

    Results are presented of investigations into the composition, uniformity and gamma-ray imaging performance of new ceramic scintillators with synthetic garnet structure. The ceramic scintillators were produced by a process that uses flame pyrolysis to make nanoparticles which are sintered into a ceramic and then compacted by hot isostatic compression into a transparent material. There is concern that the resulting ceramic scintillator might not have the uniformity of composition necessary for use in gamma-ray spectroscopy and gamma-ray imaging. The compositional uniformity of four samples of three ceramic scintillator types (GYGAG:Ce, GLuGAG:Ce and LuAG:Pr) was tested using an electron microprobe. It was found that all samples were uniform in elemental composition to the limit of sensitivity of the microprobe (few tenths of a percent atomic) over distance scales from ~ 1 cm to ~ 1 um. The light yield and energy resolution of all ceramic scintillator samples were mapped with a highly collimated 57Co source (122 keV) and performance was uniform at mapping scale of 0.25 mm. Good imaging performance with single gamma-ray photon detection was demonstrated for all samples using a BazookaSPECT system, and the imaging spatial resolution, measured as the FWHM of a LSF was 150 um.

  17. Copper uptake, intracellular localization, and speciation in marine microalgae measured by synchrotron radiation X-ray fluorescence and absorption microspectroscopy

    DOE PAGES

    Adams, Merrin S.; Dillon, Carolyn T.; Vogt, Stefan; ...

    2016-07-20

    Metal toxicity to aquatic organisms depends on the speciation of the metal and its binding to the critical receptor site(s) (biotic ligand) of the organism. The intracellular nature of the biotic ligand for Cu in microalgal cells was investigated using the high elemental sensitivity of microprobe synchrotron radiation X-ray fluorescence (SR-XRF) and X-ray absorption near-edge spectroscopy (XANES). The marine microalgae, Ceratoneis closterium, Phaeodactylum tricornutum, and Tetraselmis sp. were selected based on their varying sensitivities to Cu (72-h 50% population growth inhibitions of 8–47 μg Cu/L). Intracellular Cu in control cells was similar for all three species (2.5–3.2 × 10–15 gmore » Cu/cell) and increased 4-fold in C. closterium and Tetraselmis sp. when exposed to copper, but was unchanged in P. tricornutum (72-h exposure to 19, 40, and 40 μg Cu/L, respectively). Whole cell microprobe SR-XRF identified endogenous Cu in the central compartment (cytoplasm) of control (unexposed) cells. After Cu exposure, Cu was colocated with organelles/granules dense in P, S, Ca, and Si and this was clearly evident in thin sections of Tetraselmis sp. XANES indicated coexistence of Cu(I) and Cu(II) in control and Cu-exposed cells, with the Cu ligand (e.g., phytochelatin) in P. tricornutum different from that in C. closterium and Tetraselmis sp. Here, this study supports the hypothesis that Cu(II) is reduced to Cu(I) and that polyphosphate bodies and phytochelatins play a significant role in the internalization and detoxification of Cu in marine microalgae.« less

  18. Electron and fluorescence spectra of a water molecule irradiated by an x-ray free-electron laser pulse

    NASA Astrophysics Data System (ADS)

    Schäfer, Julia M.; Inhester, Ludger; Son, Sang-Kil; Fink, Reinhold F.; Santra, Robin

    2018-05-01

    With the highly intense x-ray light generated by x-ray free-electron lasers (XFELs), molecular samples can be ionized many times in a single pulse. Here we report on a computational study of molecular spectroscopy at the high x-ray intensity provided by XFELs. Calculated photoelectron, Auger electron, and x-ray fluorescence spectra are presented for a single water molecule that reaches many electronic hole configurations through repeated ionization steps. The rich details shown in the spectra depend on the x-ray pulse parameters in a nonintuitive way. We discuss how the observed trends can be explained by the competition of microscopic electronic transition processes. A detailed comparison between spectra calculated within the independent-atom model and within the molecular-orbital framework highlights the chemical sensitivity of the spectral lines of multiple-hole configurations. Our results demonstrate how x-ray multiphoton ionization-related effects such as charge-rearrangement-enhanced x-ray ionization of molecules and frustrated absorption manifest themselves in the electron and fluorescence spectra.

  19. Phase relations in the system Cu-Ho-O and stability of Cu{sub 2}Ho{sub 2}O{sub 5}

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

    Matthews, T.; Jacob, K.T.

    1994-01-01

    The phase relations in the system Cu-Ho-O have been determined at 1300 K using X-ray diffraction, optical microscopy, and electron microprobe analysis of samples equilibrated in evacuated quartz ampules and in pure oxygen. Only one ternary compound, Cu{sub 2}Ho{sub 2}O{sub 5}, was found to be stable. The Gibbs free energy of formation of this compound has been measured. Since the formation is endothermic, Cu{sub 2}Ho{sub 2}O{sub 5} becomes thermodynamically unstable with respect to CuO and Ho{sub 2}O{sub 3} below 810 K. When the oxygen partial pressure over Cu{sub 2}Ho{sub 2}O{sub 5} is lowered, it decomposes. The decomposition temperature at anmore » oxygen partial pressure of 1.52 X 10{sup 4} Pa was measured using a combined DTA-TGA apparatus. Based on these results, an oxygen potential diagram for the system Cu-Ho-O at 1300 K is presented.« less

  20. Hydrothermal Diamond Anvil Cell (HDAC): From Visual Observation to X-ray Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Bassett, W. A.; Mibe, K.

    2006-05-01

    A fluid sample contained in a Re gasket between two diamond anvils can be subjected to pressures up to 2.5 GPa and temperatures up to 1200°C in a resistively heated hydrothermal diamond anvil cell (HDAC). Thermocouples are used to measure temperature. The constant-volume sample chamber permits isochoric measurements that can be used to determine pressure from the equation of state of H2O and to map phases and properties in P-T space. A movie of reactions between K-feldspar and water up to 2.5 GPa and 880°C illustrates the use of visual observations for mapping coexisting solution, melt, and solid phases. X-ray absorption spectroscopy of ZnBr2 in solution up to 500°C and 500 MPa shows hydrogen bond breaking in the hydration shells of the ZnBr42- and Br- ions with increasing temperature. In other studies the stability field of ikaite (CaCO3·6H2O) has been mapped by visual observation and Raman spectroscopy; the phases of montmorillonite have been mapped by X-ray diffraction; and the leaching of Pb from zircon has been measured by X-ray microprobe.

  1. Petrology and Mineral Chemistry of New Olivine-Phyric Shergottite RBT04262

    NASA Technical Reports Server (NTRS)

    Dalton, H. A.; Peslier, A. H.; Brandon, A. D.; Lee, C.-T. A.; Lapen, T. J.

    2008-01-01

    RBT04262 was found by the 2004-2005 ANSMET team at the Roberts Massif in Antarctica. It is paired with RBT04261 and is classified as an olivine-phyric shergottite. RBT04261 is 4.0 x 3.5 x 2.5 cm and 78.8 g, and RBT04262 is 6.5 x 5.5 x 3.5 cm and 204.6 g. Both were partially covered by a fusion crust [1]. Chemical analysis and mapping of this meteorite was performed using the Cameca SX100 electron microprobe at NASA Johnson Space Center.

  2. Performance optimization of a bendable parabolic cylinder collimating X-ray mirror for the ALS micro-XAS beamline 10.3.2

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

    Yashchuk, Valeriy V.; Morrison, Gregory Y.; Marcus, Matthew A.

    The Advanced Light Source (ALS) beamline (BL) 10.3.2 is an apparatus for X-ray microprobe spectroscopy and diffraction experiments, operating in the energy range 2.4–17 keV. The performance of the beamline, namely the spatial and energy resolutions of the measurements, depends significantly on the collimation quality of light incident on the monochromator. In the BL 10.3.2 end-station, the synchrotron source is imaged 1:1 onto a set of roll slits which form a virtual source. The light from this source is collimated in the vertical direction by a bendable parabolic cylinder mirror. Details are presented of the mirror design, which allows formore » precision assembly, alignment and shaping of the mirror, as well as for extending of the mirror operating lifetime by a factor of ~10. Assembly, mirror optimal shaping and preliminary alignment were performed ex situ in the ALS X-ray Optics Laboratory (XROL). Using an original method for optimal ex situ characterization and setting of bendable X-ray optics developed at the XROL, a root-mean-square (RMS) residual surface slope error of 0.31 µrad with respect to the desired parabola, and an RMS residual height error of less than 3 nm were achieved. Once in place at the beamline, deviations from the designed optical geometry ( e.g. due to the tolerances for setting the distance to the virtual source, the grazing incidence angle, the transverse position) and/or mirror shape ( e.g. due to a heat load deformation) may appear. Due to the errors, on installation the energy spread from the monochromator is typically a few electron-volts. Here, a new technique developed and successfully implemented for at-wavelength ( in situ) fine optimal tuning of the mirror, enabling us to reduce the collimation-induced energy spread to ~0.05 eV, is described.« less

  3. Performance optimization of a bendable parabolic cylinder collimating X-ray mirror for the ALS micro-XAS beamline 10.3.2

    PubMed Central

    Yashchuk, Valeriy V.; Morrison, Gregory Y.; Marcus, Matthew A.; Domning, Edward E.; Merthe, Daniel J.; Salmassi, Farhad; Smith, Brian V.

    2015-01-01

    The Advanced Light Source (ALS) beamline (BL) 10.3.2 is an apparatus for X-ray microprobe spectroscopy and diffraction experiments, operating in the energy range 2.4–17 keV. The performance of the beamline, namely the spatial and energy resolutions of the measurements, depends significantly on the collimation quality of light incident on the monochromator. In the BL 10.3.2 end-station, the synchrotron source is imaged 1:1 onto a set of roll slits which form a virtual source. The light from this source is collimated in the vertical direction by a bendable parabolic cylinder mirror. Details are presented of the mirror design, which allows for precision assembly, alignment and shaping of the mirror, as well as for extending of the mirror operating lifetime by a factor of ∼10. Assembly, mirror optimal shaping and preliminary alignment were performed ex situ in the ALS X-ray Optics Laboratory (XROL). Using an original method for optimal ex situ characterization and setting of bendable X-ray optics developed at the XROL, a root-mean-square (RMS) residual surface slope error of 0.31 µrad with respect to the desired parabola, and an RMS residual height error of less than 3 nm were achieved. Once in place at the beamline, deviations from the designed optical geometry (e.g. due to the tolerances for setting the distance to the virtual source, the grazing incidence angle, the transverse position) and/or mirror shape (e.g. due to a heat load deformation) may appear. Due to the errors, on installation the energy spread from the monochromator is typically a few electron-volts. Here, a new technique developed and successfully implemented for at-wavelength (in situ) fine optimal tuning of the mirror, enabling us to reduce the collimation-induced energy spread to ∼0.05 eV, is described. PMID:25931083

  4. Performance optimization of a bendable parabolic cylinder collimating X-ray mirror for the ALS micro-XAS beamline 10.3.2

    DOE PAGES

    Yashchuk, Valeriy V.; Morrison, Gregory Y.; Marcus, Matthew A.; ...

    2015-04-08

    The Advanced Light Source (ALS) beamline (BL) 10.3.2 is an apparatus for X-ray microprobe spectroscopy and diffraction experiments, operating in the energy range 2.4–17 keV. The performance of the beamline, namely the spatial and energy resolutions of the measurements, depends significantly on the collimation quality of light incident on the monochromator. In the BL 10.3.2 end-station, the synchrotron source is imaged 1:1 onto a set of roll slits which form a virtual source. The light from this source is collimated in the vertical direction by a bendable parabolic cylinder mirror. Details are presented of the mirror design, which allows formore » precision assembly, alignment and shaping of the mirror, as well as for extending of the mirror operating lifetime by a factor of ~10. Assembly, mirror optimal shaping and preliminary alignment were performed ex situ in the ALS X-ray Optics Laboratory (XROL). Using an original method for optimal ex situ characterization and setting of bendable X-ray optics developed at the XROL, a root-mean-square (RMS) residual surface slope error of 0.31 µrad with respect to the desired parabola, and an RMS residual height error of less than 3 nm were achieved. Once in place at the beamline, deviations from the designed optical geometry ( e.g. due to the tolerances for setting the distance to the virtual source, the grazing incidence angle, the transverse position) and/or mirror shape ( e.g. due to a heat load deformation) may appear. Due to the errors, on installation the energy spread from the monochromator is typically a few electron-volts. Here, a new technique developed and successfully implemented for at-wavelength ( in situ) fine optimal tuning of the mirror, enabling us to reduce the collimation-induced energy spread to ~0.05 eV, is described.« less

  5. A scanning proton microprobe study of stinging emergences from the leaf of the common stinging nettle urtica dioica l.

    NASA Astrophysics Data System (ADS)

    Hughes, N. P.; Perry, C. C.; Williams, R. J. P.; Watt, F.; Grime, G. W.

    1988-03-01

    Proton-induced X-ray emission (PIXE) combined with the Oxford scanning proton microprobe (SPM) was used to investigate the abundance and spatial distribution of inorganic elements in mineralising stinging emergences from the leaf of the Common Stinging Nettle, Urtica dioica L. Elemental maps and point analytical data were collected for emergences at two stages of maturity. In all emergences calcium and silicon were spatially organised and present at high concentration. The inorganic elements K, P, S and Mn were also spatially organised during mineralisation, but at maturity these elements were present only at background levels and then showed no specific localisation. The observed changes in the inorganic content of the emergences are obviously related to the mineralisation processes. The possible biochemical significance of the distribution of the elements is discussed.

  6. As-Received, Ozone Cleaned and Ar+ Sputtered Surfaces of Hafnium Oxide Grown by Atomic Layer Deposition and Studied by XPS

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

    Engelhard, Mark H.; Herman, Jacob A.; Wallace, Robert

    2012-06-27

    In this study, X-ray photoelectron spectroscopy (XPS) characterization was performed on 47 nm thick hafnium oxide (HfO{sub 2}) films grown by atomic layer deposition using TEMA-Hf/H{sub 2}O at 250 C substrate temperature. HfO{sub 2} is currently being studied as a possible replacement for Silicon Oxide (SiO{sub 2}) as a gate dielectric in electronics transistors. XPS spectra were collected on a Physical Electronics Quantum 2000 Scanning ESCA Microprobe using a monochromatic Al K{sub a} X-ray (1486.7 eV) excitation source. The sample was analyzed under the following conditions: as received, after UV irradiation for five minutes, and after sputter cleaning with 2more » kV Ar{sup +} ions for 180 seconds. Survey scans showed carbon, oxygen, and hafnium as the major species in the film, while the only minor species of argon and carbide was detected after sputtering. Adventitious carbon initially composed approximately 18.6 AT% of the surface, but after UV cleaning it was reduced to 2.4 AT%. This demonstrated that that the majority of carbon was due to adventitious carbon. However, after 2 kV Ar{sup +} sputtering there was still only trace amounts of carbon at {approx}1 AT%, Some of this trace carbon is now in the form of a carbide due to the interaction with Ar{sup +} used for sputter cleaning. Furthermore, the stoiciometric ratio of oxygen and hafnium is consistent with a high quality HfO{sub 2} film.« less

  7. Investigation of the hard x-ray background in backlit pinhole imagers.

    PubMed

    Fein, J R; Peebles, J L; Keiter, P A; Holloway, J P; Klein, S R; Kuranz, C C; Manuel, M J-E; Drake, R P

    2014-11-01

    Hard x-rays from laser-produced hot electrons (>10 keV) in backlit pinhole imagers can give rise to a background signal that decreases signal dynamic range in radiographs. Consequently, significant uncertainties are introduced to the measured optical depth of imaged plasmas. Past experiments have demonstrated that hard x-rays are produced when hot electrons interact with the high-Z pinhole substrate used to collimate the softer He-α x-ray source. Results are presented from recent experiments performed on the OMEGA-60 laser to further study the production of hard x-rays in the pinhole substrate and how these x-rays contribute to the background signal in radiographs. Radiographic image plates measured hard x-rays from pinhole imagers with Mo, Sn, and Ta pinhole substrates. The variation in background signal between pinhole substrates provides evidence that much of this background comes from x-rays produced in the pinhole substrate itself. A Monte Carlo electron transport code was used to model x-ray production from hot electrons interacting in the pinhole substrate, as well as to model measurements of x-rays from the irradiated side of the targets, recorded by a bremsstrahlung x-ray spectrometer. Inconsistencies in inferred hot electron distributions between the different pinhole substrate materials demonstrate that additional sources of hot electrons beyond those modeled may produce hard x-rays in the pinhole substrate.

  8. Investigation of the hard x-ray background in backlit pinhole imagers

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

    Fein, J. R., E-mail: jrfein@umich.edu; Holloway, J. P.; Peebles, J. L.

    Hard x-rays from laser-produced hot electrons (>10 keV) in backlit pinhole imagers can give rise to a background signal that decreases signal dynamic range in radiographs. Consequently, significant uncertainties are introduced to the measured optical depth of imaged plasmas. Past experiments have demonstrated that hard x-rays are produced when hot electrons interact with the high-Z pinhole substrate used to collimate the softer He-α x-ray source. Results are presented from recent experiments performed on the OMEGA-60 laser to further study the production of hard x-rays in the pinhole substrate and how these x-rays contribute to the background signal in radiographs. Radiographicmore » image plates measured hard x-rays from pinhole imagers with Mo, Sn, and Ta pinhole substrates. The variation in background signal between pinhole substrates provides evidence that much of this background comes from x-rays produced in the pinhole substrate itself. A Monte Carlo electron transport code was used to model x-ray production from hot electrons interacting in the pinhole substrate, as well as to model measurements of x-rays from the irradiated side of the targets, recorded by a bremsstrahlung x-ray spectrometer. Inconsistencies in inferred hot electron distributions between the different pinhole substrate materials demonstrate that additional sources of hot electrons beyond those modeled may produce hard x-rays in the pinhole substrate.« less

  9. Miniaturized High-Speed Modulated X-Ray Source

    NASA Technical Reports Server (NTRS)

    Gendreau, Keith C. (Inventor); Arzoumanian, Zaven (Inventor); Kenyon, Steven J. (Inventor); Spartana, Nick Salvatore (Inventor)

    2015-01-01

    A miniaturized high-speed modulated X-ray source (MXS) device and a method for rapidly and arbitrarily varying with time the output X-ray photon intensities and energies. The MXS device includes an ultraviolet emitter that emits ultraviolet light, a photocathode operably coupled to the ultraviolet light-emitting diode that emits electrons, an electron multiplier operably coupled to the photocathode that multiplies incident electrons, and an anode operably coupled to the electron multiplier that is configured to produce X-rays. The method for modulating MXS includes modulating an intensity of an ultraviolet emitter to emit ultraviolet light, generating electrons in response to the ultraviolet light, multiplying the electrons to become more electrons, and producing X-rays by an anode that includes a target material configured to produce X-rays in response to impact of the more electrons.

  10. Development of a Tender-Energy Microprobe for Geosciences at NSLS and NSLS-II

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

    Northrup, Paul A.

    This funding is to develop a new Synchrotron user facility for microbeam X-ray absorption spectroscopy (XAS) and quantitative X-ray fluorescence (XRF) imaging, at the National Synchrotron Light Source (NSLS) and NSLS-II. It includes design, purchase of components, and construction of the microprobe endstation and controls. Initial development, commissioning, and application is ongoing at NSLS Beamline X15B, with planned transition in 2014-15 to the NSLS-II TES (Tender-Energy Spatially Resolved X-ray Absorption Spectroscopy) beamline. It is optimized for the “tender” energy range of 1-5 keV, reaching up to 8 keV. Thus it uniquely covers the K absorption edges of critical elements Mg,more » Al, Si, P, S, Cl, and Ca, and can reach up to Co. A stable, high-flux microbeam focus, user-tunable from ~50 to ~5 microns, has been achieved using two-stage achromatic focusing. Existing beamline optics collimate, monochromate, and macro-focus the X-ray beam to ~1 mm at a secondary source aperture (SSA). Beam from the SSA is then re-focused by a pair of mirrors in KB geometry to the microbeam scale. Size of the microbeam is tunable, at the expense of flux, by adjusting the size of the SSA as a virtual source. The new experimental endstation consists of 1) a sample chamber operable as a radiation enclosure with helium atmosphere to facilitate measurements in this energy range, 2) the KB microfocusing optics, 3) a sample-positioning stage for raster-scanning and positioning the sample, 4) X-ray fluorescence detectors, an existing Ge detector for low-signal sensitivity and a new Si detector for high count rates, 5) an optical camera for viewing samples and locating target locations, 6) beam intensity monitors and diagnostics, and 7) controls and data acquisition system. An important aspect of this project is the added capability for fast, on-the-fly scanning of the monochromator (energy), required for fast XAS and advanced XAS imaging. This instrument will be available for initial PI and Co-I measurements, and for General Users to apply for beamtime to use, at NSLS X15B for the remaining operation of NSLS, to September 30, 2014. Phase two of this project will transition this facility, both the primary optics and the endstation, to NSLS-II after NSLS ceases operation. While this transition itself is beyond the scope of the current grant, preparation and planning for it is included.« less

  11. Note: Measurement of the runaway electrons in the J-TEXT tokamak

    NASA Astrophysics Data System (ADS)

    Chen, Z. Y.; Zhang, Y.; Zhang, X. Q.; Luo, Y. H.; Jin, W.; Li, J. C.; Chen, Z. P.; Wang, Z. J.; Yang, Z. J.; Zhuang, G.

    2012-05-01

    The runaway electrons have been measured by hard x-ray detectors and soft x-ray array in the J-TEXT tokamak. The hard x-ray radiations in the energy ranges of 0.5-5 MeV are measured by two NaI detectors. The flux of lost runaway electrons can be obtained routinely. The soft x-ray array diagnostics are used to monitor the runaway beam generated in disruptions since the soft x-ray is dominated by the interaction between runaway electrons and metallic impurities inside the plasma. With the aid of soft x-ray array, runaway electron beam has been detected directly during the formation of runaway current plateau following the disruptions.

  12. CT Colonography (Virtual Colonoscopy)

    MedlinePlus

    ... Rotating around you, the x-ray tube and electronic x-ray detectors are located opposite each other ... numerous x-ray beams and a set of electronic x-ray detectors rotate around you, measuring the ...

  13. Synthesis and characterization of P-doped amorphous and nanocrystalline Si

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

    Wang, Jialing; Ganguly, Shreyashi; Sen, Sabyasachi

    Intentional impurity doping lies at the heart of the silicon technology. The dopants provide electrons or holes as necessary carriers of the electron current and can significantly modify the electric, optical and magnetic properties of the semiconductors. P-doped amorphous Si (a-Si) was prepared by a solid state and solution metathesis reaction of a P-doped Zintl phase precursor, NaSi 0.99P 0.01, with an excess of NH 4X (X = Br, I). After the salt byproduct was removed from the solid state reaction, the a-Si material was annealed at 600 °C under vacuum for 2 h, resulting in P-doped nanocrystalline Si (nc-Si)more » material embedded in a-Si matrix. The product from the solution reaction also shows a combination of nc-Si embedded in a-Si; however, it was fully converted to nc-Si after annealing under argon at 650 °C for 30 min. Powder X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM) show the amorphous nature of the P-doped Si material before the annealing and the nanocrystallinity after the annealing. Fourier Transform Infrared (FTIR) spectroscopy shows that the P-doped Si material surface is partially capped by H and O or with solvent. Finally, electron microprobe wavelength dispersive spectroscopy (WDS) as well as energy dispersive spectroscopy (EDS) confirm the presence of P in the Si material. 29Si and 31P solid state magic-angle-spinning nuclear magnetic resonance (MAS NMR) spectroscopy data provide the evidence of P doping into the Si structure with the P concentration of approximately 0.07 at.%.« less

  14. Structural and compositional characterization of synthetic (Ca,Sr)-tremolite and (Ca,Sr)-diopside solid solutions

    NASA Astrophysics Data System (ADS)

    Gottschalk, M.; Najorka, J.; Andrut, M.

    Tremolite (CaxSr1-x)2Mg5[Si8O22/(OH)2] and diopside (CaxSr1-x)Mg[Si2O6] solid solutions have been synthesized hydrothermally in equilibrium with a 1 molar (Ca,Sr)Cl2 aqueous solution at 750°C and 200 MPa. The solid run products have been investigated by optical, electron scanning and high resolution transmission electron microscopy, electron microprobe, X-ray-powder diffraction and Fourier-transform infrared spectroscopy. The synthesized (Ca,Sr)-tremolites are up to 2000 µm long and 30 µm wide, the (Ca,Sr)-diopsides are up to 150 µm long and 20 µm wide. In most runs the tremolites and diopsides are well ordered and chain multiplicity faults are rare. Nearly pure Sr-tremolite (tr0.02Sr-tr0.98) and Sr-diopside (di0.01Sr-di0.99) have been synthesized. A continuous solid solution series, i.e. complete substitution of Sr2+ for Ca2+ on M4-sites exists for (Ca,Sr)-tremolite. Total substitution of Sr2+ for Ca2+ on M2-sites can be assumed for (Ca,Sr)-diopsides. For (Ca,Sr)-tremolites the lattice parameters a, b and β are linear functions of composition and increase with Sr-content whereas c is constant. For the diopside series all 4 lattice parameters are a linear function of composition; a, b, c increase and β decreases with rising Sr-content. The unit cell volume for tremolite increases 3.47% from 906.68 Å3 for tremolite to 938.21 Å3 for Sr-tremolite. For diopside the unit cell volume increases 4.87 % from 439.91 Å3 for diopside to 461.30 Å3 for Sr-diopside. The observed splitting of the OH stretching band in tremolite is caused by different configurations of the next nearest neighbors (multi mode behavior). Resolved single bands can be attributed to the following configurations on the M4-sites: SrSr, SrCa, CaCa and CaMg. The peak positions of these 4 absorption bands are a linear function of composition. They are shifted to lower wavenumbers with increasing Sr-content. No absorption band due to the SrMg configuration on the M4-site is observed. This indicates a very low or negligible cummingtonite component in Sr-rich tremolites, which is also supported by electron microprobe analysis.

  15. ONR (Office of Naval Research) Far East Scientific Information Bulletin. Volume 13, Number 4, October-December 1988

    DTIC Science & Technology

    1988-12-01

    by light finger pressure; and surface shaded or rubbed by soft pencil, charcoal, or crayon. Anglers initiated this custom as a means of recording...related to the barium titanate or simple nects, and mixers. Some of these applica- perovskite unit cell (Figure 1). In this struc- tions can be...dispersive spectroscopy (EDS), Target-~ microprobe analysis, and x-ray diffraction R~orOC(XRD). MagnetsOptical microscopy with polarized light

  16. Antiferromagnetic-ferromagnetic crossover in UO 2-TiO x multi-phase systems

    NASA Astrophysics Data System (ADS)

    Nakamura, Akio; Tsutsui, Satoshi; Yoshii, Kenji

    2001-05-01

    An antiferromagnetic (AF)-weakly ferromagnetic (WF) crossover has been found for UO 2-TiO x multi-phase systems, (1- y)UO 2+ yTiO x ( y=0.05-0.72, x=0, 1.0, 1.5 and 2.0), when these mixtures are heat treated at high temperature in vacuum. From the powder X-ray diffraction and electron-microprobe analyses, their phase assemblies were as follows: for x=0, 1.0 and 1.5, a heterogeneous two-phase mixture of UO 2+TiO x; for x=2.0, that of UO 2+UTi 2O 6 for y<0.67, showing characteristic microstructures, and for y>0.67 that of UTi 2O 6+TiO 2 (plus residual minor UO 2). Magnetic susceptibility ( χ) of the present UO 2 powder was confirmed to exhibit an antiferromagnetic sharp drop at TN (=30.5 K). In contrast, χ of these multi-phase systems was found to exhibit a sharp upturn at the respective TN, while their TN values remained almost constant with varying y. This χ upturn at TN is most pronounced for UO 2+Ti-oxide (titania) systems ( x=1.0, 1.5 and 2.0) over the wide mixture ratio above y˜0.10. These observations indicate that an AF-WF crossover is induced for these multi-phase systems, plausibly due to the interfacial magnetic modification of UO 2 in contact with the oxide partners.

  17. In-situ determination of metallic variation and multi-association in single particles by combining synchrotron microprobe, sequential chemical extraction and multivariate statistical analysis.

    PubMed

    Zhu, Yu-Min; Zhang, Hua; Fan, Shi-Suo; Wang, Si-Jia; Xia, Yi; Shao, Li-Ming; He, Pin-Jing

    2014-07-15

    Due to the heterogeneity of metal distribution, it is challenging to identify the speciation, source and fate of metals in solid samples at micro scales. To overcome these challenges single particles of air pollution control residues were detected in situ by synchrotron microprobe after each step of chemical extraction and analyzed by multivariate statistical analysis. Results showed that Pb, Cu and Zn co-existed as acid soluble fractions during chemical extraction, regardless of their individual distribution as chlorides or oxides in the raw particles. Besides the forms of Fe2O3, MnO2 and FeCr2O4, Fe, Mn, Cr and Ni were closely associated with each other, mainly as reducible fractions. In addition, the two groups of metals had interrelations with the Si-containing insoluble matrix. The binding could not be directly detected by micro-X-ray diffraction (μ-XRD) and XRD, suggesting their partial existence as amorphous forms or in the solid solution. The combined method on single particles can effectively determine metallic multi-associations and various extraction behaviors that could not be identified by XRD, μ-XRD or X-ray absorption spectroscopy. The results are useful for further source identification and migration tracing of heavy metals. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Earth, soil and environmental science research facility at sector 13 of the Advanced Photon Source. II. Scientific program and experimental instrumentation (abstract)

    NASA Astrophysics Data System (ADS)

    Sutton, S.; Eng., P. J.; Jaski, Y. R.; Lazaraz, N.; Pluth, J.; Murray, P.; Rarback, H.; Rivers, M.

    1996-09-01

    The GSECARS (APS sector 13) scientific program will provide fundamental new information on the deep structure and composition of the Earth and other planets, the formation of economic mineral deposits, the cycles and fate of toxic metals in the environment, and the mechanisms of nutrient uptake and disease in plants. In the four experimental stations (2 per beamline), scientists will have access to three main x-ray techniques: diffraction (microcrystal, powder, diamond anvil cell, and large volume press), fluorescence microprobe, and spectroscopy (conventional, microbeam, liquid and solid surfaces). The high pressure facilities will be capable of x-ray crystallography at P≳360 GPa and T˜6000 K with the diamond anvil cell and P˜25 GPa and T˜2500 °C with the large volume press. Diffractometers will allow study of 1 micrometer crystals and micro-powders. The microprobe (1 micrometer focused beam) will be capable of chemical analyses in the sub-ppm range using wavelength and energy dispersive detectors. Spectroscopy instrumentation will be available for XANES and EXAFS with microbeams as well as high sensitivity conventional XAS and studies of liquid and solid interfaces. Visiting scientists will be able to setup, calibrate, and test experiments in off-line laboratories with equipment such as micromanipulators, optical microscopes, clean bench, glove boxes, high powered optical and Raman spectrometers.

  19. Few-femtosecond time-resolved measurements of X-ray free-electron lasers.

    PubMed

    Behrens, C; Decker, F-J; Ding, Y; Dolgashev, V A; Frisch, J; Huang, Z; Krejcik, P; Loos, H; Lutman, A; Maxwell, T J; Turner, J; Wang, J; Wang, M-H; Welch, J; Wu, J

    2014-04-30

    X-ray free-electron lasers, with pulse durations ranging from a few to several hundred femtoseconds, are uniquely suited for studying atomic, molecular, chemical and biological systems. Characterizing the temporal profiles of these femtosecond X-ray pulses that vary from shot to shot is not only challenging but also important for data interpretation. Here we report the time-resolved measurements of X-ray free-electron lasers by using an X-band radiofrequency transverse deflector at the Linac Coherent Light Source. We demonstrate this method to be a simple, non-invasive technique with a large dynamic range for single-shot electron and X-ray temporal characterization. A resolution of less than 1 fs root mean square has been achieved for soft X-ray pulses. The lasing evolution along the undulator has been studied with the electron trapping being observed as the X-ray peak power approaches 100 GW.

  20. Development of scanning electron and x-ray microscope

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

    Matsumura, Tomokazu, E-mail: tomokzau.matsumura@etd.hpk.co.jp; Hirano, Tomohiko, E-mail: tomohiko.hirano@etd.hpk.co.jp; Suyama, Motohiro, E-mail: suyama@etd.hpk.co.jp

    We have developed a new type of microscope possessing a unique feature of observing both scanning electron and X-ray images under one unit. Unlike former X-ray microscopes using SEM [1, 2], this scanning electron and X-ray (SELX) microscope has a sample in vacuum, thus it enables one to observe a surface structure of a sample by SEM mode, to search the region of interest, and to observe an X-ray image which transmits the region. For the X-ray observation, we have been focusing on the soft X-ray region from 280 eV to 3 keV to observe some bio samples and softmore » materials. The resolutions of SEM and X-ray modes are 50 nm and 100 nm, respectively, at the electron energy of 7 keV.« less

  1. Characterization of the Basalt of Broken Tank, NM for the 'in situ' Calibration Target for the Alpha-Particle X-ray Spectrometer (APXS) on the Upcoming Mars Science Laboratory (MSL) Rover

    NASA Astrophysics Data System (ADS)

    Burkemper, L.; King, P. L.; Gellert, R.; Spilde, M. N.; Chamberlin, R. M.

    2008-12-01

    The MSL rover mission will launch in Fall 2009. It is equipped with an APXS for analyzing the bulk chemistry of rocks and soils. To monitor the APXS performance in situ on the martian surface over the extended mission, a calibration target will be included on the MSL rover. Engineering constraints led to a 4.2 cm diameter, 3 mm thick, homogeneous rock disc that would survive vibrations during launch. The basalt from Broken Tank, NM was chosen for the flight disc from ~200 volcanic rocks. The basalt is relatively homogeneous, fine- and even-grained, vesicle-free, and extremely dense and hard due to its ophitic texture. Other volcanic rocks - even well characterized samples of BCR - were ruled out due to vesicles, or high contents of glass, phenocrysts, secondary minerals, or fractures. The flight disc was prepared by hand- polishing to a 0.05 micron finish. We obtained scanning electron microscope back-scattered electron maps and X-ray maps (Al, Mg, Ca, Fe, Ti, Na, and K) on the polished, uncoated surface of the target. One pit (~0.03 mm2) and three tiny surface imperfections (<0.04 mm2) were observed on the surface. Electron microprobe analyses on two C-coated thin sections give the following compositions: olivine cores Fa23Fo77 and rims Fa40Fo60; plagioclase cores Ab42An56Or2 and discrete rims Ab62An7Or31; oxides Ilm67Hm33 and also trace chromite, apatite, chlorite, clays and devitrified glass. The NIH software Scion Image was used to determine the modal abundance of each phase in the basalt disk and in two thin sections. Bulk composition was established with multiple XRF laboratory analyses. There is no significant heterogeneity on the scale of the APXS analysis (~1.5 cm). Sulfides were not observed and XRF verified low Ni (<90 ppm) and S (70 ppm), making these elements ideal to monitor any Martian dust build-up during the surface operation. The rock slab is glued into a Ni frame, mounted vertically and accessible with a brush tool. The K- and L- X-ray lines of Ni can be used to monitor the energy efficiency of the X-ray detector. This work was supported by the Space Science Enhancement Program of the Canadian Space Agency and the New Mexico Space Grant Consortium.

  2. Pore-Scale Characterization of Biogeochemical Controls on Iron and Uranium Speciation under Flow Conditions

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

    Pearce, Carolyn I.; Wilkins, Michael J.; Zhang, Changyong

    2012-09-17

    Etched silicon microfluidic pore network models (micromodels) with controlled chemical and redox gradients, mineralogy, and microbiology under continuous flow conditions are used for the incremental development of complex microenvironments that simulate subsurface conditions. We demonstrate the colonization of micromodel pore spaces by an anaerobic Fe(III)-reducing bacterial species (Geobacter sulfurreducens) and the enzymatic reduction of a bioavailable Fe(III) phase within this environment. Using both X-ray Microprobe and X-ray Absorption Spectroscopy, we investigate the combined effects of the precipitated Fe(III) phases and the microbial population on uranium biogeochemistry under flow conditions. Precipitated Fe(III) phases within the micromodel were most effectively reduced inmore » the presence of an electron shuttle (AQDS), and Fe(II) ions adsorbed onto the precipitated mineral surface without inducing any structural change. In the absence of Fe(III), U(VI) was effectively reduced by the microbial population to insoluble U(IV), which was precipitated in discrete regions associated with biomass. In the presence of Fe(III) phases, however, both U(IV) and U(VI) could be detected associated with biomass, suggesting re-oxidation of U(IV) by localized Fe(III) phases. These results demonstrate the importance of the spatial localization of biomass and redox active metals, and illustrate the key effects of pore-scale processes on contaminant fate and reactive transport.« less

  3. Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

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

    Kersell, Heath; Shirato, Nozomi; Cummings, Marvin

    We use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated and therebymore » the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens a new avenue for materials characterization on a one particle at-a-time basis.« less

  4. Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

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

    Kersell, Heath; Shirato, Nozomi; Cummings, Marvin

    Here, we use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated andmore » thereby the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens a new avenue for materials characterization on a one particle at-a-time basis.« less

  5. Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

    DOE PAGES

    Kersell, Heath; Shirato, Nozomi; Cummings, Marvin; ...

    2017-09-05

    Here, we use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated andmore » thereby the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens a new avenue for materials characterization on a one particle at-a-time basis.« less

  6. Examination of Surveyor 3 parts with the scanning electron microscope and electron microprobe

    NASA Technical Reports Server (NTRS)

    Chodos, A. A.; Devaney, J. R.; Evens, K. C.

    1972-01-01

    Two screws and two washers, several small chips of tubing, and a fiber removed from a third screw were examined with the scanning electron microscope and the electron microprobe. The purpose of the examination was to determine the nature of the material on the surface of these samples and to search for the presence of meteoritic material.

  7. Improved normal tissue protection by proton and X-ray microchannels compared to homogeneous field irradiation.

    PubMed

    Girst, S; Marx, C; Bräuer-Krisch, E; Bravin, A; Bartzsch, S; Oelfke, U; Greubel, C; Reindl, J; Siebenwirth, C; Zlobinskaya, O; Multhoff, G; Dollinger, G; Schmid, T E; Wilkens, J J

    2015-09-01

    The risk of developing normal tissue injuries often limits the radiation dose that can be applied to the tumour in radiation therapy. Microbeam Radiation Therapy (MRT), a spatially fractionated photon radiotherapy is currently tested at the European Synchrotron Radiation Facility (ESRF) to improve normal tissue protection. MRT utilizes an array of microscopically thin and nearly parallel X-ray beams that are generated by a synchrotron. At the ion microprobe SNAKE in Munich focused proton microbeams ("proton microchannels") are studied to improve normal tissue protection. Here, we comparatively investigate microbeam/microchannel irradiations with sub-millimetre X-ray versus proton beams to minimize the risk of normal tissue damage in a human skin model, in vitro. Skin tissues were irradiated with a mean dose of 2 Gy over the irradiated area either with parallel synchrotron-generated X-ray beams at the ESRF or with 20 MeV protons at SNAKE using four different irradiation modes: homogeneous field, parallel lines and microchannel applications using two different channel sizes. Normal tissue viability as determined in an MTT test was significantly higher after proton or X-ray microchannel irradiation compared to a homogeneous field irradiation. In line with these findings genetic damage, as determined by the measurement of micronuclei in keratinocytes, was significantly reduced after proton or X-ray microchannel compared to a homogeneous field irradiation. Our data show that skin irradiation using either X-ray or proton microchannels maintain a higher cell viability and DNA integrity compared to a homogeneous irradiation, and thus might improve normal tissue protection after radiation therapy. Copyright © 2015 Associazione Italiana di Fisica Medica. Published by Elsevier Ltd. All rights reserved.

  8. Nuclear microprobe investigation of the penetration of ultrafine zinc oxide into intact and tape-stripped human skin

    NASA Astrophysics Data System (ADS)

    Szikszai, Z.; Kertész, Zs.; Bodnár, E.; Major, I.; Borbíró, I.; Kiss, Á. Z.; Hunyadi, J.

    2010-06-01

    Ultrafine metal oxides, such as titanium dioxide and zinc oxide are widely used in cosmetic and health products like sunscreens. These oxides are potent UV filters and the small particle size makes the product more transparent compared to formulations containing coarser particles. In the present work the penetration of ultrafine zinc oxide into intact and tape-stripped human skin was investigated using nuclear microprobe techniques, such as proton induced X-ray spectroscopy and scanning transmission ion microscopy. Our results indicate that the penetration of ultrafine zinc oxide, in a hydrophobic basis gel with 48 h application time, is limited to the stratum corneum layer of the intact skin. Removing the stratum corneum partially or entirely by tape-stripping did not cause the penetration of the particles into the deeper dermal layers; the zinc particles remained on the surface of the skin.

  9. Laboratory Scale X-ray Fluorescence Tomography: Instrument Characterization and Application in Earth and Environmental Science.

    PubMed

    Laforce, Brecht; Vermeulen, Bram; Garrevoet, Jan; Vekemans, Bart; Van Hoorebeke, Luc; Janssen, Colin; Vincze, Laszlo

    2016-03-15

    A new laboratory scale X-ray fluorescence (XRF) imaging instrument, based on an X-ray microfocus tube equipped with a monocapillary optic, has been developed to perform XRF computed tomography experiments with both higher spatial resolution (20 μm) and a better energy resolution (130 eV @Mn-K(α)) than has been achieved up-to-now. This instrument opens a new range of possible applications for XRF-CT. Next to the analytical characterization of the setup by using well-defined model/reference samples, demonstrating its capabilities for tomographic imaging, the XRF-CT microprobe has been used to image the interior of an ecotoxicological model organism, Americamysis bahia. This had been exposed to elevated metal (Cu and Ni) concentrations. The technique allowed the visualization of the accumulation sites of copper, clearly indicating the affected organs, i.e. either the gastric system or the hepatopancreas. As another illustrative application, the scanner has been employed to investigate goethite spherules from the Cretaceous-Paleogene boundary, revealing the internal elemental distribution of these valuable distal ejecta layer particles.

  10. Evaluation of the diffusion of Mn, Fe, Ba and Pb in Middle Ages human teeth by synchrotron microprobe X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Carvalho, M. L.; Marques, A. F.; Marques, J. P.; Casaca, C.

    2007-07-01

    Human teeth from the Middle Ages have been analysed using a synchrotron microprobe evaluating Mn, Fe, Ba and Pb diffusion from the soil into the tooth structure. It is apparent that post-mortem teeth of ancient populations are influenced by the endogenous environment. The diffusion pattern of some elements can give information both for archaeological purposes and diagenesis processes affecting the apatite ante-mortem elemental content. An X-ray fluorescence set-up with microprobe capabilities, 100 μm of spatial resolution and energy of 18 keV, installed at LURE synchrotron (France) was used. Line scans were performed along the several regions of the teeth, in steps of 100 to 1000 μm. Ba is much enriched in ancient teeth when compared to recent ones, where this element is almost non-existent. Furthermore, the concentration profiles show increased levels of this element close to the external enamel region, reaching values up to 200 μg g - 1 decreasing in dentine and achieving a steady level in the inner dentine and root. Pb concentration profiles show strongly increased levels of this element close to the external enamel region (20 μg g - 1 ), decreasing strongly to the inner part of the dentine (0.5 μg g - 1 ) contrarily to the normal situation in modern citizens where the highest concentrations for Pb are in the inner root dentine. This behaviour suggests post-mortem uptake from the soil; the presence of elevated levels of Pb can be explained by the fact that this burial place was a car park for more than 20 years. The distribution of Mn and Fe follow very similar patterns and both are very much enriched especially in the outer surfaces in contact with the soil, showing strong contamination from the soil.

  11. Correlated petrographic, electron microprobe, and ion microprobe studies of selected primitive and processed phase assemblages in meteorites

    NASA Technical Reports Server (NTRS)

    Albee, Arden L.

    1993-01-01

    During the past three years we have received support to continue our research in elucidating the formation and alteration histories of selected meteoritic materials by a combination of petrographic, trace element, and isotopic analyses employing optical and scanning electron microscopes and electron and ion microprobes. The awarded research funds enabled the P.I. to attend the annual LPSC, the co-I to devote approximately 15 percent of his time to the research proposed in the grant, and partial support for a visiting summer post-doctoral fellow to conduct electron microprobe analyses of meteoritic samples in our laboratory. The research funds, along with support from the NASA Education Initiative awarded to P.I. G. Wasserburg, enabled the co-I to continue a mentoring program with inner-city minority youth. The support enabled us to achieve significant results in the five projects that we proposed (in addition to the Education Initiative), namely: studies of the accretional and post-accretional alteration and thermal histories in CV meteorites, characterization of periclase-bearing Fremdlinge in CV meteorites, characterization of Ni-Pt-Ge-Te-rich Fremdlinge in CV meteorites in an attempt to determine the constraints they place on the petrogenetic and thermal histories of their host CAI's, correlated electron and ion microprobe studies of silicate and phosphate inclusions in the Colomera meteorite in an attempt to determine the petrogenesis of the IE iron meteorites, and development of improved instrumental and correction procedures for improved accuracy of analysis of meteoritic materials with the electron microprobe. This grant supported, in part or whole, 18 publications so far by our research team, with at least three more papers anticipated. The list of these publications is included. The details of the research results are briefly summarized.

  12. THz-pump and X-ray-probe sources based on an electron linac

    NASA Astrophysics Data System (ADS)

    Setiniyaz, Sadiq; Park, Seong Hee; Kim, Hyun Woo; Vinokurov, Nikolay A.; Jang, Kyu-Ha; Lee, Kitae; Baek, In Hyung; Jeong, Young Uk

    2017-11-01

    We describe a compact THz-pump and X-ray-probe beamline, based on an electron linac, for ultrafast time-resolved diffraction applications. Two high-energy electron (γ > 50) bunches, 5 ns apart, impinge upon a single-foil or multifoil radiator and generate THz radiation and X-rays simultaneously. The THz pulse from the first bunch is synchronized to the X-ray beam of the second bunch by using an adjustable optical delay of a THz pulse. The peak power of THz radiation from the multifoil radiator is estimated to be 0.14 GW for a 200 pC well-optimized electron bunch. GEANT4 simulations show that a carbon foil with a thickness of 0.5-1.0 mm has the highest yield of 10-20 keV hard X-rays for a 25 MeV beam, which is approximately 103 photons/(keV pC-electrons) within a few degrees of the polar angle. A carbon multifoil radiator with 35 foils (25 μm thick each) can generate close to 103 hard X-rays/(keV pC-electrons) within a 2° acceptance angle. With 200 pC charge and a 100 Hz repetition rate, we can generate 107 X-rays per 1 keV energy bin per second or 105 X-rays per 1 keV energy bin per pulse. The longitudinal time profile of an X-ray pulse ranges from 400 to 600 fs depending on the acceptance angle. The broadening of the time duration of an X-ray pulse is observed owing to its diverging effect. A double-crystal monochromator will be used to select and transport the desired X-rays to the sample. The heating of the radiators by an electron beam is negligible because of the low beam current.

  13. Miniature, low-power X-ray tube using a microchannel electron generator electron source

    NASA Technical Reports Server (NTRS)

    Elam, Wm. Timothy (Inventor); Kelliher, Warren C. (Inventor); Hershyn, William (Inventor); DeLong, David P. (Inventor)

    2011-01-01

    Embodiments of the invention provide a novel, low-power X-ray tube and X-ray generating system. Embodiments of the invention use a multichannel electron generator as the electron source, thereby increasing reliability and decreasing power consumption of the X-ray tube. Unlike tubes using a conventional filament that must be heated by a current power source, embodiments of the invention require only a voltage power source, use very little current, and have no cooling requirements. The microchannel electron generator comprises one or more microchannel plates (MCPs), Each MCP comprises a honeycomb assembly of a plurality of annular components, which may be stacked to increase electron intensity. The multichannel electron generator used enables directional control of electron flow. In addition, the multichannel electron generator used is more robust than conventional filaments, making the resulting X-ray tube very shock and vibration resistant.

  14. Ultrafast Science Opportunities with Electron Microscopy

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

    Durr, Hermann

    X-rays and electrons are two of the most fundamental probes of matter. When the Linac Coherent Light Source (LCLS), the world’s first x-ray free electron laser, began operation in 2009, it transformed ultrafast science with the ability to generate laser-like x-ray pulses from the manipulation of relativistic electron beams. This document describes a similar future transformation. In Transmission Electron Microscopy, ultrafast relativistic (MeV energy) electron pulses can achieve unsurpassed spatial and temporal resolution. Ultrafast temporal resolution will be the next frontier in electron microscopy and can ideally complement ultrafast x-ray science done with free electron lasers. This document describes themore » Grand Challenge science opportunities in chemistry, material science, physics and biology that arise from an MeV ultrafast electron diffraction & microscopy facility, especially when coupled with linac-based intense THz and X-ray pump capabilities.« less

  15. Compton spectra of atoms at high x-ray intensity

    NASA Astrophysics Data System (ADS)

    Son, Sang-Kil; Geffert, Otfried; Santra, Robin

    2017-03-01

    Compton scattering is the nonresonant inelastic scattering of an x-ray photon by an electron and has been used to probe the electron momentum distribution in gas-phase and condensed-matter samples. In the low x-ray intensity regime, Compton scattering from atoms dominantly comes from bound electrons in neutral atoms, neglecting contributions from bound electrons in ions and free (ionized) electrons. In contrast, in the high x-ray intensity regime, the sample experiences severe ionization via x-ray multiphoton multiple ionization dynamics. Thus, it becomes necessary to take into account all the contributions to the Compton scattering signal when atoms are exposed to high-intensity x-ray pulses provided by x-ray free-electron lasers (XFELs). In this paper, we investigate the Compton spectra of atoms at high x-ray intensity, using an extension of the integrated x-ray atomic physics toolkit, xatom. As the x-ray fluence increases, there is a significant contribution from ionized electrons to the Compton spectra, which gives rise to strong deviations from the Compton spectra of neutral atoms. The present study provides not only understanding of the fundamental XFEL-matter interaction but also crucial information for single-particle imaging experiments, where Compton scattering is no longer negligible. , which features invited work from the best early-career researchers working within the scope of J. Phys. B. This project is part of the Journal of Physics series’ 50th anniversary celebrations in 2017. Sang-Kil Son was selected by the Editorial Board of J. Phys. B as an Emerging Leader.

  16. RF Phase Stability and Electron Beam Characterization for the PLEIADES Thomson X-Ray Source

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

    Brown, W J; Hartemann, F V; Tremaine, A M

    2002-10-16

    We report on the performance of an S-band RF photocathode electron gun and accelerator for operation with the PLEIADES Thomson x-ray source at LLNL. To produce picosecond, high brightness x-ray pulses, picosecond timing, terahertz bandwidth diagnostics, and RF phase control are required. Planned optical, RF, x-ray and electron beam measurements to characterize the dependence of electron beam parameters and synchronization on RF phase stability are presented.

  17. Millimeter, microwave, hard X-ray, and soft X-ray observations of energetic electron populations in solar flares

    NASA Technical Reports Server (NTRS)

    Kundu, M. R.; White, S. M.; Gopalswamy, N.; Lim, J.

    1994-01-01

    We present comparisons of multiwavelength data for a number of solar flares observed during the major campaign of 1991 June. The different wavelengths are diagnostics of energetic electrons in different energy ranges: soft X-rays are produced by electrons with energies typically below 10 keV, hard X-rays by electrons with energies in the range 10-200 keV, microwaves by electrons in the range 100 keV-1 MeV, and millimeter-wavelength emission by electrons with energies of 0.5 MeV and above. The flares in the 1991 June active period were remarkable in two ways: all have very high turnover frequencies in their microwave spectra, and very soft hard X-ray spectra. The sensitivity of the microwave and millimeter data permit us to study the more energetic (greater than 0.3 MeV) electrons even in small flares, where their high-energy bremsstrahlung is too weak for present detectors. The millimeter data show delays in the onset of emission with respect to the emissions associated with lower energy electrons and differences in time profiles, energy spectral indices incompatible with those implied by the hard X-ray data, and a range of variability of the peak flux in the impulsive phase when compared with the peak hard X-ray flux which is two orders of magnitude larger than the corresponding variability in the peak microwave flux. All these results suggest that the hard X-ray-emitting electrons and those at higher energies which produce millimeter emission must be regarded as separate populations. This has implications for the well-known 'number problem' found previously when comparing the numbers of non thermal electrons required to produce the hard X-ray and radio emissions.

  18. Femtosecond profiling of shaped x-ray pulses

    NASA Astrophysics Data System (ADS)

    Hoffmann, M. C.; Grguraš, I.; Behrens, C.; Bostedt, C.; Bozek, J.; Bromberger, H.; Coffee, R.; Costello, J. T.; DiMauro, L. F.; Ding, Y.; Doumy, G.; Helml, W.; Ilchen, M.; Kienberger, R.; Lee, S.; Maier, A. R.; Mazza, T.; Meyer, M.; Messerschmidt, M.; Schorb, S.; Schweinberger, W.; Zhang, K.; Cavalieri, A. L.

    2018-03-01

    Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fully suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. This achievement completes an important step toward future x-ray pulse shaping techniques.

  19. High-intensity double-pulse X-ray free-electron laser

    DOE PAGES

    Marinelli, A.; Ratner, D.; Lutman, A. A.; ...

    2015-03-06

    The X-ray free-electron laser has opened a new era for photon science, improving the X-ray brightness by ten orders of magnitude over previously available sources. Similar to an optical laser, the spectral and temporal structure of the radiation pulses can be tailored to the specific needs of many experiments by accurately manipulating the lasing medium, that is, the electron beam. Here we report the generation of mJ-level two-colour hard X-ray pulses of few femtoseconds duration with an XFEL driven by twin electron bunches at the Linac Coherent Light Source. This performance represents an improvement of over an order of magnitudemore » in peak power over state-of-the-art two-colour XFELs. The unprecedented intensity and temporal coherence of this new two-colour X-ray free-electron laser enable an entirely new set of scientific applications, ranging from X-ray pump/X-ray probe experiments to the imaging of complex biological samples with multiple wavelength anomalous dispersion.« less

  20. Compton backscattered collimated x-ray source

    DOEpatents

    Ruth, R.D.; Huang, Z.

    1998-10-20

    A high-intensity, inexpensive and collimated x-ray source is disclosed for applications such as x-ray lithography is disclosed. An intense pulse from a high power laser, stored in a high-finesse resonator, repetitively collides nearly head-on with and Compton backscatters off a bunched electron beam, having relatively low energy and circulating in a compact storage ring. Both the laser and the electron beams are tightly focused and matched at the interaction region inside the optical resonator. The laser-electron interaction not only gives rise to x-rays at the desired wavelength, but also cools and stabilizes the electrons against intrabeam scattering and Coulomb repulsion with each other in the storage ring. This cooling provides a compact, intense bunch of electrons suitable for many applications. In particular, a sufficient amount of x-rays can be generated by this device to make it an excellent and flexible Compton backscattered x-ray (CBX) source for high throughput x-ray lithography and many other applications. 4 figs.

  1. Compton backscattered collimated x-ray source

    DOEpatents

    Ruth, Ronald D.; Huang, Zhirong

    1998-01-01

    A high-intensity, inexpensive and collimated x-ray source for applications such as x-ray lithography is disclosed. An intense pulse from a high power laser, stored in a high-finesse resonator, repetitively collides nearly head-on with and Compton backscatters off a bunched electron beam, having relatively low energy and circulating in a compact storage ring. Both the laser and the electron beams are tightly focused and matched at the interaction region inside the optical resonator. The laser-electron interaction not only gives rise to x-rays at the desired wavelength, but also cools and stabilizes the electrons against intrabeam scattering and Coulomb repulsion with each other in the storage ring. This cooling provides a compact, intense bunch of electrons suitable for many applications. In particular, a sufficient amount of x-rays can be generated by this device to make it an excellent and flexible Compton backscattered x-ray (CBX) source for high throughput x-ray lithography and many other applications.

  2. Compton backscattered collmated X-ray source

    DOEpatents

    Ruth, Ronald D.; Huang, Zhirong

    2000-01-01

    A high-intensity, inexpensive and collimated x-ray source for applications such as x-ray lithography is disclosed. An intense pulse from a high power laser, stored in a high-finesse resonator, repetitively collides nearly head-on with and Compton backscatters off a bunched electron beam, having relatively low energy and circulating in a compact storage ring. Both the laser and the electron beams are tightly focused and matched at the interaction region inside the optical resonator. The laser-electron interaction not only gives rise to x-rays at the desired wavelength, but also cools and stabilizes the electrons against intrabeam scattering and Coulomb repulsion with each other in the storage ring. This cooling provides a compact, intense bunch of electrons suitable for many applications. In particular, a sufficient amount of x-rays can be generated by this device to make it an excellent and flexible Compton backscattered x-ray (CBX) source for high throughput x-ray lithography and many other applications.

  3. Stabilized phosphogypsum: class C fly ash: Portland type II cement composites for potential marine application.

    PubMed

    Guo, T; Malone, R F; Rusch, K A

    2001-10-01

    Phosphogypsum (PG, CaSO4 x H20), a byproduct of phosphoric acid manufacturing, contains low levels of Ra226. PG can be stabilized with portland type II cement and class C fly ash for use in marine environments, thus eliminating the airborne vector of transmission for radon gas. An augmented simplex centroid design with pseudocomponents was used to select 10 PG:class C fly ash:portland type II cement compositions. The 43 cm3 blocks were fabricated and subjected to a 1.5-yr field submergence test and a 28-d saltwater dynamic leaching study. All field composites survived with no signs of degradation. Dynamic leaching resulted in effective calcium diffusion coefficients ranging from 0.21 to 7.5 x 10(-14)m2 s(-1). Effective diffusion depths, calculated for t=1 and 30 yr, ranged from 0.4 to 2.2 mm and from 2.0 to 11.9 mm, respectively. Scanning electron microscopy and wavelength dispersive microprobe and X-ray diffraction analyses of the leached composites identified a 40-60-microm calcite layer that was absent in the control composites. This suggests that a reaction between the composites and the saltwater results in the precipitation of calcite onto the block surface, encapsulating the composites and protecting them from saltwater attack and dissolution.

  4. Generation of first hard X-ray pulse at Tsinghua Thomson Scattering X-ray Source.

    PubMed

    Du, Yingchao; Yan, Lixin; Hua, Jianfei; Du, Qiang; Zhang, Zhen; Li, Renkai; Qian, Houjun; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

    2013-05-01

    Tsinghua Thomson Scattering X-ray Source (TTX) is the first-of-its-kind dedicated hard X-ray source in China based on the Thomson scattering between a terawatt ultrashort laser and relativistic electron beams. In this paper, we report the experimental generation and characterization of the first hard X-ray pulses (51.7 keV) via head-on collision of an 800 nm laser and 46.7 MeV electron beams. The measured yield is 1.0 × 10(6) per pulse with an electron bunch charge of 200 pC and laser pulse energy of 300 mJ. The angular intensity distribution and energy spectra of the X-ray pulse are measured with an electron-multiplying charge-coupled device using a CsI scintillator and silicon attenuators. These measurements agree well with theoretical and simulation predictions. An imaging test using the X-ray pulse at the TTX is also presented.

  5. Structure flexibility of the Cu2ZnSnS4 absorber in low-cost photovoltaic cells: from the stoichiometric to the copper-poor compounds.

    PubMed

    Choubrac, L; Lafond, A; Guillot-Deudon, C; Moëlo, Y; Jobic, S

    2012-03-19

    Here we present for the very first time a single-crystal investigation of the Cu-poor Zn-rich derivative of Cu(2)ZnSnS(4). Nowadays, this composition is considered as the one that delivers the best photovoltaic performances in the specific domain of Cu(2)ZnSnS(4)-based thin-film solar cells. The existence of this nonstoichiometric phase is definitely demonstrated here in an explicit and unequivocal manner on the basis of powder and single-crystal X-ray diffraction analyses coupled with electron microprobe analyses. Crystals are tetragonal, space group I ̅4, Z = 2, with a = 5.43440(15) Å and c = 10.8382(6) Å for Cu(2)ZnSnS(4) and a = 5.43006(5) Å and c = 10.8222(2) Å for Cu(1.71)Zn(1.18)Sn(0.99)S(4). © 2012 American Chemical Society

  6. Hot corrosion evaluation of aluminide coated superalloys in support of an ASTM Round Robin program

    NASA Technical Reports Server (NTRS)

    Santoro, G.

    1975-01-01

    Commercial aluminized coatings on substrates were hot corroded at 900 C in a 0.3 Mach burner rig with 5 ppm synthetic sea salt and at two cycling frequencies. Extensive post-exposure examinations were conducted on the corroded specimens such as metallography, X-ray diffraction, scanning electron microscopy, microprobe raster scans, and spectrographic analyses. Thermodynamic calculations were made of the equilibrium burner flame composition and the calculations were compared to the experimental findings. It was found that localized spalling of the coatings preceded coating failure. It is suggested that the spalling of the coatings is due to the formation of localized stresses caused by the depletion of chromium and aluminum in the coating or the enrichment of the coating with sulfur. For the materials and test conditions investigated, it was found that coating life is dependent only upon the initial coating thickness and not on the type of aluminized coating, the substrate, or the cycle frequency.

  7. Aluminium alloys in municipal solid waste incineration bottom ash.

    PubMed

    Hu, Yanjun; Rem, Peter

    2009-05-01

    With the increasing growth of incineration of household waste, more and more aluminium is retained in municipal solid waste incinerator bottom ash. Therefore recycling of aluminium from bottom ash becomes increasingly important. Previous research suggests that aluminium from different sources is found in different size fractions resulting in different recycling rates. The purpose of this study was to develop analytical and sampling techniques to measure the particle size distribution of individual alloys in bottom ash. In particular, cast aluminium alloys were investigated. Based on the particle size distribution it was computed how well these alloys were recovered in a typical state-of-the-art treatment plant. Assessment of the cast alloy distribution was carried out by wet physical separation processes, as well as chemical methods, X-ray fluorescence analysis and electron microprobe analysis. The results from laboratory analyses showed that cast alloys tend to concentrate in the coarser fractions and therefore are better recovered in bottom ash treatment plants.

  8. Relationship of Optical Anomalies, Zoning, and Microtopography in Vesuvianite from Jeffrey Mine, Asbestos, Quebec

    NASA Astrophysics Data System (ADS)

    Smith, Varina Campbell

    The role of growth steps in inducing disequilibrium is investigated in crystals of vesuvianite from the Jeffrey mine, Asbestos, Quebec, using optical microscopy, atomic force microscopy, electron microprobe analysis, and single-crystal X-ray diffraction. The selective uptake of elements Fe and Al by asymmetric growth-steps on three crystallographic forms, {100}, {110}, and {121}, is documented. The prisms {100} and {110} show hillocks that display kinetically controlled oscillatory zoning along growth steps parallel to <010> and <11¯1>, but not on vicinal faces defined by [001] steps. Sector-specific zoning of extinction angles and 2V angles indicate different degrees of optical dissymmetrization in crystals spanning a range of growth habits. Unit-cell parameters and the presence of violating reflections confirm sectoral deviations from P4/nnc symmetry in the prismatic sectors. The partial loss of three glide planes follows the pattern expected from order of the cations Al and Fe induced by tangential selectivity at the edge of non-equivalent steps during layer-by-layer growth.

  9. Impactite and pseudotachylite from Roter Kamm Crater, Namibia

    NASA Technical Reports Server (NTRS)

    Degenhardt, J. J., Jr.; Buchanan, P. C.; Reid, A. M.

    1992-01-01

    Pseudotachylite is known to occur in a variety of geologic settings including thrust belts (e.g., the Alps and the Himalayas) and impact craters such as Roter Kamm, Namibia. Controversy exists, however, as to whether pseudotachylite can be produced by shock brecciation as well as by tectonic frictional melting. Also open to debate is the question of whether pseudotachylites form by frictional fusion or by cataclasis. It was speculated that the pseudotachylite at Roter Kamm was formed by extensional settling and adjustment of basement blocks during 'late modification stage' of impact. The occurrence of pseudotachylite in association with rocks resembling quenched glass bombs and melt breccias in a relatively young crater of known impact origin offers a rare opportunity to compare features of these materials. Petrographic, x-ray diffraction, and electron microprobe analyses of the impactites and pseudotachylites are being employed to determine the modes of deformation and to assess the role of frictional melting and comminution of adjacent target rocks.

  10. The 2003 phreatomagmatic eruptions of Anatahan volcano - Textural and petrologic features of deposits at an emergent island volcano

    USGS Publications Warehouse

    Pallister, J.S.; Trusdell, F.A.; Brownfield, I.K.; Siems, D.F.; Budahn, J.R.; Sutley, S.F.

    2005-01-01

    Stratigraphic and field data are used in conjunction with textural and chemical evidence (including data from scanning electron microscope, electron microprobe, X-ray fluorescence, X-ray diffraction, and instrumental neutron activation analysis) to establish that the 2003 eruption of Anatahan volcano was mainly phreatomagmatic, dominated by explosive interaction of homogeneous composition low-viscosity crystal-poor andesite magma with water. The hydromagmatic mode of eruption contributed to the significant height of initial eruptive columns and to the excavation and eruption of altered rock debris from the sub-volcanic hydrothermal system. Volatile contents of glass inclusions in equilibrium phenocrysts less abundances of these constituents in matrix glass times the estimated mass of juvenile magma indicate minimum emissions of 19 kt SO2 and 13 kt Cl. This petrologic estimate of SO2 emission is an order-of-magnitude less than an estimate from TOMS. Similarly, inferred magma volumes from the petrologic data are an order of magnitude greater than those modeled from deformation data. Both discrepancies indicate additional sources of volatiles, likely derived from a separate fluid phase in the magma. The paucity of near-source volcanic-tectonic earthquakes preceding the eruption, and the dominance of sustained long-period tremor are attributed to the ease of ascent of the hot low-viscosity andesite, followed by a shallow phreatomagmatic mode of eruption. Phreatomagmatic eruptions are probably more common at emergent tropical island volcanoes, where shallow fresh-water lenses occur at near-sea-level vents. These relations suggest that phreatomagmatic explosions contributed to the formation of many of the near-sea-level craters and possibly even to the small calderas at the other Mariana islands.

  11. Nonlinear X-Ray and Auger Spectroscopy at X-Ray Free-Electron Laser Sources

    NASA Astrophysics Data System (ADS)

    Rohringer, Nina

    2015-05-01

    X-ray free-electron lasers (XFELs) open the pathway to transfer non-linear spectroscopic techniques to the x-ray domain. A promising all x-ray pump probe technique is based on coherent stimulated electronic x-ray Raman scattering, which was recently demonstrated in atomic neon. By tuning the XFEL pulse to core-excited resonances, a few seed photons in the spectral tail of the XFEL pulse drive an avalanche of resonant inelastic x-ray scattering events, resulting in exponential amplification of the scattering signal by of 6-7 orders of magnitude. Analysis of the line profile of the emitted radiation permits to demonstrate the cross over from amplified spontaneous emission to coherent stimulated resonance scattering. In combination with statistical covariance mapping, a high-resolution spectrum of the resonant inelastic scattering process can be obtained, opening the path to coherent stimulated x-ray Raman spectroscopy. An extension of these ideas to molecules and a realistic feasibility study of stimulated electronic x-ray Raman scattering in CO will be presented. Challenges to realizing stimulated electronic x-ray Raman scattering at present-day XFEL sources will be discussed, corroborated by results of a recent experiment at the LCLS XFEL. Due to the small gain cross section in molecular targets, other nonlinear spectroscopic techniques such as nonlinear Auger spectroscopy could become a powerful alternative. Theory predictions of a novel pump probe technique based on resonant nonlinear Auger spectroscopic will be discussed and the method will be compared to stimulated x-ray Raman spectroscopy.

  12. X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

    NASA Astrophysics Data System (ADS)

    Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

    2018-06-01

    X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

  13. Seeing Atoms and Molecules in Action with an Electron 'Eye' | Berkeley Lab

    Science.gov Websites

    , also called "electron guns," that can drive advanced X-ray lasers known as "free form of X-ray light. Free-electron lasers have opened new frontiers in studying materials and chemistry that you can look at with an X-ray free-electron laser, but with an electron eye." He added, "

  14. X-ray tube with magnetic electron steering

    DOEpatents

    Reed, Kim W.; Turman, Bobby N.; Kaye, Ronald J.; Schneider, Larry X.

    2000-01-01

    An X-ray tube uses a magnetic field to steer electrons. The magnetic field urges electrons toward the anode, increasing the proportion of electrons emitted from the cathode that reach desired portions of the anode and consequently contribute to X-ray production. The magnetic field also urges electrons reflected from the anode back to the anode, further increasing the efficiency of the tube.

  15. Macroscopic and molecular-scale assessment of soil lead contamination impacted by seasonal dove hunting activities

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

    Arai, Y.; Tappero, R.; Rick, A.R.

    Environmental contamination of lead (Pb) in soils and sediments poses serious threats to human and ecological health. The objective of this study is to investigate the effect of seasonal dove sports hunting activities on Pb contamination in acid forest soils. A grid sampling method was used to investigate the spatial distribution of Pb contamination in surface soils. Soils were analyzed for total metal(loid) concentration and characterized for physicochemical properties and mineralogy. Adsorption isotherm experiments were also conducted to understand the reactivity and retention capacity of Pb(II) in soils. Finally, synchrotron-based X-ray microprobe and X-ray absorption spectroscopy were used to understandmore » the chemical speciation of Pb that controls the retention/release mechanisms of Pb in soils. There was no excessive accumulation of Pb at the site. However, the concentration of Pb in surface soils was greater than the background level (<16 mg kg{sup -1}). The contamination level of Pb was as high as 67 mg kg{sup -1} near a patch of corn field where lime was frequently applied. A microfocused X-ray microprobe analysis showed the presence of Pb pellet fragments that predominantly contain oxidized Pb(II), suggesting that oxidative dissolution was occurring in soils. Dissolved Pb(II) can be readily retained in soils up to {approx}3,600 mg kg{sup -1} via inner-sphere and outer-sphere surface complexation on carbon and aluminol functional groups of soil components, suggesting that partitioning reactions control the concentration of Pb in soil solution. The fate of Pb is likely to be controlled by (1) oxidative dissolution process of Pb(0) pellets and (2) the release of outer-sphere and/or inner-sphere Pb surface complexes in humic substances and aluminosilicate/Al oxyhydroxides. Although no remedial actions are immediately required, the long-term accumulation of Pb in soils should be carefully monitored in protecting ecosystem and water quality at the dove hunting field.« less

  16. High-pressure studies with x-rays using diamond anvil cells

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

    Shen, Guoyin; Mao, Ho Kwang

    2016-11-22

    Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials' properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. Thesemore » HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.« less

  17. High-pressure studies with x-rays using diamond anvil cells

    NASA Astrophysics Data System (ADS)

    Shen, Guoyin; Mao, Ho Kwang

    2017-01-01

    Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials’ properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. These HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.

  18. Miniaturized, High-Speed, Modulated X-Ray Source

    NASA Technical Reports Server (NTRS)

    Gendreau, Keith; Arzoumanian, Zaven; Kenyon, Steve; Spartana, Nick

    2013-01-01

    A low-cost, miniature x-ray source has been developed that can be modulated in intensity from completely off to full intensity on nanosecond timescales. This modulated x-ray source (MXS) has no filaments and is extremely rugged. The energy level of the MXS is adjustable from 0 to more than 100 keV. It can be used as the core of many new devices, providing the first practical, arbitrarily time-variable source of x-rays. The high-speed switching capability and miniature size make possible many new technologies including x-ray-based communication, compact time-resolved x-ray diffraction, novel x-ray fluorescence instruments, and low- and precise-dose medical x-rays. To make x-rays, the usual method is to accelerate electrons into a target material held at a high potential. When the electrons stop in the target, x-rays are produced with a spectrum that is a function of the target material and the energy to which the electrons are accelerated. Most commonly, the electrons come from a hot filament. In the MXS, the electrons start off as optically driven photoelectrons. The modulation of the x-rays is then tied to the modulation of the light that drives the photoelectron source. Much of the recent development has consisted of creating a photoelectrically-driven electron source that is robust, low in cost, and offers high intensity. For robustness, metal photocathodes were adopted, including aluminum and magnesium. Ultraviolet light from 255- to 350-nm LEDs (light emitting diodes) stimulated the photoemissions from these photocathodes with an efficiency that is maximized at the low-wavelength end (255 nm) to a value of roughly 10(exp -4). The MXS units now have much higher brightness, are much smaller, and are made using a number of commercially available components, making them extremely inexpensive. In the latest MXS design, UV efficiency is addressed by using a high-gain electron multiplier. The photocathode is vapor-deposited onto the input cone of a Burle Magnum(TradeMark) multiplier. This system yields an extremely robust photon-driven electron source that can tolerate long, weeks or more, exposure to air with negligible degradation. The package is also small. When combined with the electron target, necessary vacuum fittings, and supporting components (but not including LED electronics or high-voltage sources), the entire modulated x-ray source weighs as little as 158 grams.

  19. Use of geochemical mass balance modelling to evaluate the role of weathering in determining stream chemistry in five mid-Atlantic watersheds on different lithologies

    USGS Publications Warehouse

    O'Brien, Anne K.; Rice, Karen C.; Bricker, Owen P.; Kennedy, Margaret M.; Anderson, R. Todd

    1997-01-01

    The importance of mineral weathering was assessed and compared for five mid-Atlantic watersheds receiving similar atmospheric inputs but underlain by differing bedrock. Annual solute mass balances and volume-weighted mean solute concentrations were calculated for each watershed for each year of record. In addition, primary and secondary mineralogy were determined for each of the watersheds through analysis of soil samples and thin sections using petrographic, scanning electron microscope, electron microprobe and X-ray diffraction techniques. Mineralogical data were also compiled from the literature. These data were input to NETPATH, a geochemical program that calculates the masses of minerals that react with precipitation to produce stream water chemistry. The feasibilities of the weathering scenarios calculated by NETPATH were evaluated based on relative abundances and reactivities of minerals in the watershed. In watersheds underlain by reactive bedrocks, weathering reactions explained the stream base cation loading. In the acid-sensitive watersheds on unreactive bedrock, calculated weathering scenarios were not consistent with the abundance of reactive minerals in the underlying bedrock, and alternative sources of base cations are discussed.

  20. Magnesium degradation influenced by buffering salts in concentrations typical of in vitro and in vivo models.

    PubMed

    Agha, Nezha Ahmad; Feyerabend, Frank; Mihailova, Boriana; Heidrich, Stefanie; Bismayer, Ulrich; Willumeit-Römer, Regine

    2016-01-01

    Magnesium and its alloys have considerable potential for orthopedic applications. During the degradation process the interface between material and tissue is continuously changing. Moreover, too fast or uncontrolled degradation is detrimental for the outcome in vivo. Therefore in vitro setups utilizing physiological conditions are promising for the material/degradation analysis prior to animal experiments. The aim of this study is to elucidate the influence of inorganic salts contributing to the blood buffering capacity on degradation. Extruded pure magnesium samples were immersed under cell culture conditions for 3 and 10 days. Hank's balanced salt solution without calcium and magnesium (HBSS) plus 10% of fetal bovine serum (FBS) was used as the basic immersion medium. Additionally, different inorganic salts were added with respect to concentration in Dulbecco's modified Eagle's medium (DMEM, in vitro model) and human plasma (in vivo model) to form 12 different immersion media. Influences on the surrounding environment were observed by measuring pH and osmolality. The degradation interface was analyzed by electron-induced X-ray emission (EIXE) spectroscopy, including chemical-element mappings and electron microprobe analysis, as well as Fourier transform infrared reflection micro-spectroscopy (FTIR). Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Attenuation of heavy metals by geosynthetics in the coal gangue-filled columns.

    PubMed

    Wang, Ping; Hu, Zhenqi; Wang, Peijun

    2013-01-01

    In the subsided areas backfilled with coal gangue, an issue of continuing environmental concern is the migration of hazardous metals to the subsurface soil and groundwater. As an effective isolation material, geosynthetics have been scarcely applied into mining areas reclamation of China. This paper describes research aimed at characterizing the behaviours of different geosynthetics in the leaching columns filled with coal gangues. Four types of geosynthetics were selected: fibres needle-punched nonwoven geotextiles, high-density polyethylene, needle-punched Na-bentonite geosynthetic clay liner (GCL-NP) and Na-bentonite geosynthetic-overbited film. Heavy metals were significantly attenuated and by monitoring aqueous solutions in the whole percolation period, negative correlation was found between pH value and concentration of heavy metals. Generally, GCL-NP showed comparatively better effects on attenuating the migration of heavy metals. According to the meta-analysis of heavy metals present in the leachates and retained in the columns, geosynthetics have good capabilities of sorption and retardation, which can delay the breakthrough time of heavy metals and retard the accumulation in the subsurface. Future research will use X-ray diffraction and micro-imaging (electron microprobe and scanning electron microscopy) to further explain retention mechanisms.

  2. A mineralogical study in contrasts: highly mineralized whale rostrum and human enamel

    NASA Astrophysics Data System (ADS)

    Li, Zhen; Ai-Jawad, Maisoon; Siddiqui, Samera; Pasteris, Jill D.

    2015-11-01

    The outermost enamel of the human tooth and the rostrum of the whale Mesoplodon densirostris are two highly mineralized tissues that contain over 95 wt.% mineral, i.e., bioapatite. However, the same mineral type (carbonated hydroxylapatite) does not yield the same material properties, as revealed by Raman spectroscopy, scanning electron microscopy, electron microprobe analysis, and synchrotron X-ray diffraction analysis. Overall, the outermost enamel of a tooth has more homogeneous physical and chemical features than the rostrum. Chemical comparison of rostrum and enamel shows bioapatite in the rostrum to be enriched in Na, Mg, CO3, and S, whereas the outermost enamel shows only a slightly enriched Cl concentration. Morphologically, mineral rods (at tens of μm scale), crystallites and prisms (at μm and sub-μm scale), and platelets (at tens of nm scale) all demonstrate less organized texture in the rostrum than in enamel. Such contrasts between two mineralized tissues suggest distinct pathways of biomineralization, e.g., the nature of the equilibrium between mineral and body fluid. This study illustrates the remarkable flexibility of the apatite mineral structure to match its chemical and physical properties to specific biological needs within the same animal or between species.

  3. Processings of the Workshop on Electron Contamination in X-Ray Astronomy Experiments. [proceedings of conference on effects of extraterrestrial radiation

    NASA Technical Reports Server (NTRS)

    Holt, S. S. (Editor)

    1974-01-01

    The proceedings of a conference to investigate the effects of extraterrestrial radiation and particle contamination of X-ray astronomical data are presented. The subjects discussed include the following: (1) electrons at low altitudes which affect soft X-ray astronomy, (2) the geographical distribution of 100 keV electrons above the earth's atmosphere, (3) midlatitude electron precipitation, (4) particle background observed by X-ray detectors on board Copernicus satellite, and (5) a survey of trapped low energy electrons near the inner boundary of the inner radiation zone as determined by OSO-7.

  4. X-ray fluorescence mapping of mercury on suspended mineral particles and diatoms in a contaminated freshwater system

    NASA Astrophysics Data System (ADS)

    Gu, B.; Mishra, B.; Miller, C.; Wang, W.; Lai, B.; Brooks, S. C.; Kemner, K. M.; Liang, L.

    2014-05-01

    Mercury (Hg) bioavailability and geochemical cycling is affected by its partitioning between the aqueous and particulate phases. We applied X-ray fluorescence (XRF) microprobes to directly visualize and quantify the spatial localization of Hg and its correlations with other elements of interest on suspended particles from a Hg contaminated freshwater system. Up to 175 μg g-1 Hg is found on suspended particles. Mercury is heterogeneously distributed among phytoplankton (e.g., diatoms) and mineral particles that are rich in iron oxides and natural organic matter (NOM), possibly as Hg-NOM-iron oxide ternary complexes. The diatom-bound Hg is mostly found on outer surfaces of the cells, suggesting passive sorption of inorganic Hg on diatoms. Our results indicate that localized sorption of Hg onto suspended particles, including diatoms and NOM-coated oxide minerals, is an important sink for Hg in natural aquatic environments.

  5. Hyperspectral image reconstruction for x-ray fluorescence tomography

    DOE PAGES

    Gürsoy, Doǧa; Biçer, Tekin; Lanzirotti, Antonio; ...

    2015-01-01

    A penalized maximum-likelihood estimation is proposed to perform hyperspectral (spatio-spectral) image reconstruction for X-ray fluorescence tomography. The approach minimizes a Poisson-based negative log-likelihood of the observed photon counts, and uses a penalty term that has the effect of encouraging local continuity of model parameter estimates in both spatial and spectral dimensions simultaneously. The performance of the reconstruction method is demonstrated with experimental data acquired from a seed of arabidopsis thaliana collected at the 13-ID-E microprobe beamline at the Advanced Photon Source. The resulting element distribution estimates with the proposed approach show significantly better reconstruction quality than the conventional analytical inversionmore » approaches, and allows for a high data compression factor which can reduce data acquisition times remarkably. In particular, this technique provides the capability to tomographically reconstruct full energy dispersive spectra without compromising reconstruction artifacts that impact the interpretation of results.« less

  6. Discovery of Diffuse Hard X-ray Emission associated with Jupiter

    NASA Astrophysics Data System (ADS)

    Ezoe, Y.; Miyoshi, Y.; Ishikawa, K.; Ohashi, T.; Terada, N.; Uchiyama, Y.; Negoro, H.

    2009-12-01

    Our discovery of diffuse hard (1-5 keV) X-ray emission around Jupiter is reported. Recent Chandra and XMM-Newton observations revealed several types of X-rays in the vicinity of Jupiter such as auroral and disk emission from Jupiter and faint diffuse X-rays from the Io Plasma Torus (see Bhardwaj et al. 2007 for review). To investigate possible diffuse hard X-ray emission around Jupiter with the highest sensitivity, we conducted data analysis of Suzaku XIS observations of Jupiter on Feb 2006. After removing satellite and planetary orbital motions, we detected a significant diffuse X-ray emission extending to ~6 x 3 arcmin with the 1-5 keV X-ray luminosity of ~3e15 erg/s. The emitting region very well coincided with the Jupiter's radiation belts. The 1-5 keV X-ray spectrum was represented by a simple power law model with a photon index of 1.4. Such a flat continuum strongly suggests non-thermal origin. Although such an emission can be originated from multiple background point sources, its possibility is quite low. We hence examined three mechanisms, assuming that the emission is truly diffuse: bremsstrahlung by keV electrons, synchrotron emission by TeV electrons, and inverse Compton scattering of solar photons by MeV electrons. The former two can be rejected because of the X-ray spectral shape and implausible existence of TeV electrons around Jupiter, respectively. The last possibility was found to be possible because tens MeV electrons, which have been confirmed in inner radiation belts (Bolton et al. 2002), can kick solar photons to the keV energy range and provide a simple power-law continuum. We estimated an average electron density from the X-ray luminosity assuming the oblate spheroid shaped emitting region with 8 x 8 x 4 Jovian radii. The necessary density was 0.02 1/cm3 for 50 MeV electrons. Hence, our results may suggest a new particle acceleration phenomenon around Jupiter.

  7. Femtosecond profiling of shaped x-ray pulses

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

    Hoffmann, M. C.; Grguras, I.; Behrens, C.

    Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fullymore » suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. Furthermore, this achievement completes an important step toward future x-ray pulse shaping techniques.« less

  8. Femtosecond profiling of shaped x-ray pulses

    DOE PAGES

    Hoffmann, M. C.; Grguras, I.; Behrens, C.; ...

    2018-03-26

    Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fullymore » suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. Furthermore, this achievement completes an important step toward future x-ray pulse shaping techniques.« less

  9. Attosecond time-energy structure of X-ray free-electron laser pulses

    NASA Astrophysics Data System (ADS)

    Hartmann, N.; Hartmann, G.; Heider, R.; Wagner, M. S.; Ilchen, M.; Buck, J.; Lindahl, A. O.; Benko, C.; Grünert, J.; Krzywinski, J.; Liu, J.; Lutman, A. A.; Marinelli, A.; Maxwell, T.; Miahnahri, A. A.; Moeller, S. P.; Planas, M.; Robinson, J.; Kazansky, A. K.; Kabachnik, N. M.; Viefhaus, J.; Feurer, T.; Kienberger, R.; Coffee, R. N.; Helml, W.

    2018-04-01

    The time-energy information of ultrashort X-ray free-electron laser pulses generated by the Linac Coherent Light Source is measured with attosecond resolution via angular streaking of neon 1s photoelectrons. The X-ray pulses promote electrons from the neon core level into an ionization continuum, where they are dressed with the electric field of a circularly polarized infrared laser. This induces characteristic modulations of the resulting photoelectron energy and angular distribution. From these modulations we recover the single-shot attosecond intensity structure and chirp of arbitrary X-ray pulses based on self-amplified spontaneous emission, which have eluded direct measurement so far. We characterize individual attosecond pulses, including their instantaneous frequency, and identify double pulses with well-defined delays and spectral properties, thus paving the way for X-ray pump/X-ray probe attosecond free-electron laser science.

  10. THz-pump and X-ray-probe sources based on an electron linac.

    PubMed

    Setiniyaz, Sadiq; Park, Seong Hee; Kim, Hyun Woo; Vinokurov, Nikolay A; Jang, Kyu-Ha; Lee, Kitae; Baek, In Hyung; Jeong, Young Uk

    2017-11-01

    We describe a compact THz-pump and X-ray-probe beamline, based on an electron linac, for ultrafast time-resolved diffraction applications. Two high-energy electron (γ > 50) bunches, 5 ns apart, impinge upon a single-foil or multifoil radiator and generate THz radiation and X-rays simultaneously. The THz pulse from the first bunch is synchronized to the X-ray beam of the second bunch by using an adjustable optical delay of a THz pulse. The peak power of THz radiation from the multifoil radiator is estimated to be 0.14 GW for a 200 pC well-optimized electron bunch. GEANT4 simulations show that a carbon foil with a thickness of 0.5-1.0 mm has the highest yield of 10-20 keV hard X-rays for a 25 MeV beam, which is approximately 10 3 photons/(keV pC-electrons) within a few degrees of the polar angle. A carbon multifoil radiator with 35 foils (25 μm thick each) can generate close to 10 3 hard X-rays/(keV pC-electrons) within a 2° acceptance angle. With 200 pC charge and a 100 Hz repetition rate, we can generate 10 7 X-rays per 1 keV energy bin per second or 10 5 X-rays per 1 keV energy bin per pulse. The longitudinal time profile of an X-ray pulse ranges from 400 to 600 fs depending on the acceptance angle. The broadening of the time duration of an X-ray pulse is observed owing to its diverging effect. A double-crystal monochromator will be used to select and transport the desired X-rays to the sample. The heating of the radiators by an electron beam is negligible because of the low beam current.

  11. Growth and Electronic Structure of Heusler Compounds for Use in Electron Spin Based Devices

    DTIC Science & Technology

    2015-06-01

    either Co– or MnSi– initiated films on c(4x4) GaAs. Studies using x - ray photoemission spectroscopy (XPS), STM/STS, and transmission electron microscopy...Co– or MnSi– initiated films on c(4x4) GaAs. Studies using x - ray photoemission spectroscopy (XPS), STM/STS, and transmission electron microscopy (TEM...diagram of the Palmstrøm lab in-situ growth and char- acterization setup, with 6 MBE growth chambers, 3 scanning probe microscopes, an x - ray

  12. Multi-scale analysis of the occurrence of Pb, Cr and Mn in the NIST standards: Urban dust (SRM 1649a) and indoor dust (SRM 2584)

    NASA Astrophysics Data System (ADS)

    Jiang, Mingyu; Nakamatsu, Yuki; Jensen, Keld A.; Utsunomiya, Satoshi

    2014-01-01

    Adverse health effects of ambient particulate matters are closely related to the speciation of the constituting organic matters and toxic metals. To determine multi-parameters of the metal speciation in urban and indoor dusts, we have performed systematic bulk- to nano-scale (“multi-scale”) analysis on the speciation of Pb, Mn, and Cr in two National Institute of Standards and Technology (NIST) standard reference materials (SRMs): urban dust (SRM 1649a) and indoor dust (SRM 2584), utilizing X-ray absorption near-edge structure, powder X-ray diffraction analysis, electron microprobe analysis, scanning electron microscopy, and transmission electron microscopy. Major crystalline phases are quartz, gypsum, kaolinite, and muscovite in SRM 1649a, while quartz, gypsum, calcite, and possibly muscovite (or chabazite) in SRM 2584. A number of Pb sulfate nanoparticles (50-200 nm) occur in SRM 1649a, whereas micron-sized Pb carbonate is present containing various concentrations of Zn and Ti in the complex texture in SRM 2584. Relatively soluble Mn(II) sulfate is the bulk-averaged Mn speciation in SRM 1649a, although discrete Mn sulfate particles are not characterized by individual particle analysis, implying the diluted Mn distribution within other sulfate. In SRM 2584, Mn speciation includes a mixture of oxides and carbonates, and trace Mn in chromite. Chromite (FeCr2O4) is the major Cr speciation in SRM1694a, while unidentified Cr(III) phases with minor chromite and Pb chromate are present in SRM 2584, among which the Pb chromate is composed of Cr(VI). A significant number of the metal-bearing particles are distributed to the submicron-size fraction in the urban dust, SRM 1649a, suggesting that these metal nanoparticles can potentially penetrate into the deep respiratory system. This study demonstrates that multi-scale analysis combining nano and bulk analytical techniques is a powerful approach to investigate the multi-parameters of metal-bearing nanoparticles in heterogeneous PM samples.

  13. Long life electrodes for large-area x-ray generators

    NASA Technical Reports Server (NTRS)

    Rothe, Dietmar E. (Inventor)

    1991-01-01

    This invention is directed to rugged, reliable, and long-life electrodes for use in large-area, high-current-density electron gun and x-ray generators which are employed as contamination-free preionizers for high-energy pulsed gas lasers. The electron source at the cathode is a corona plasma formed at the interface between a conductor, or semiconductor, and a high-permittivity dielectric. Detailed descriptions are provided of a reliable cold plasma cathode, as well as an efficient liquid-cooled electron beam target (anode) and x-ray generator which concentrates the x-ray flux in the direction of an x-ray window.

  14. X-ray spectra and electron structure of A15 compounds of transition metals

    NASA Astrophysics Data System (ADS)

    Kurmaev, E. Z.; Iarmoshenko, Iu. M.

    1988-01-01

    Results of an X-ray emission spectroscopy study of the electron structure of A15 compounds are reported. In particular, attention is given to the X-ray spectra of A15 compounds of the A3B type with transition and nontransition elements, effect of alloying on the formation of the electron structure of ternary phases, and effect of atomic ordering in the X-ray spectra of A15 compounds with changes in heat treament and concentration. The X-ray spectra of A15 compounds irradiated by fast neutrons are also examined.

  15. Experimental study of Fe-Mg- and Ca-distribution between coexisting ortho- and clinopyroxenes at P=294 MPa, T=750 and 800° C

    NASA Astrophysics Data System (ADS)

    Fonarev, V. I.; Graphchikov, A. A.

    1982-07-01

    The Fe-Mg-Ca-distribution was investigated in synthesis experiments and with the mineral assemblage orthopyroxene+clinopyroxene+quartz. The phase compositions were identified by X-ray diffraction and, where possible, by electron microprobe. The attainment of equilibrium in the run products was signalled by the compositions from control runs (different solutions) becoming closely similar, by recycling runs, by the attainment of equilibrium from different directions (depending on the composition of starting phases), and by special kinetic experiments. The study produced the following results: (1) the Ca content of the clinopyroxenes decreases with increasing Fe (mol%) from 48.4 at X {Cpx/Fe}=5 to 39.8 at X {Cpx/Fe}=45 (800° C); from 47.6 at X {Cpx/Fe}= 10 to 41.7 at X {Cpx/Fe}=45 (750° C); increasing temperature expands the stability field of the less calcic clinopyroxenes. (2) The Ca content of orthopyroxenes increases slightly with Fe content from 1.8 at X {Opx/Fe}=20.5 to 3.2 at X {Opx/Fe}=75; the temperature effect on the Ca content under the T, P conditions of the experiment was not large. (3) Fe and Mg distribution between the coexisting ortho-and clinopyroxenes is largely temperature-dependent, particularly in the compositional range X {Opx/Fe}=15 75 mol%; as T increases, Fe redistributes from the rhombic to monoclinic mineral. Preliminary estimates of rock formation temperatures using the obtained data show that most of the known two-pyroxene geothermometers overstate the actual values by 50 150° C.

  16. Two types of electron events in solar flares

    NASA Technical Reports Server (NTRS)

    Daibog, E. I.; Kurt, V. G.; Logachev, Y. I.; Stolpovsky, V. G.

    1985-01-01

    The fluxes and spectra of the flare electrons measured on board Venera-I3 and I4 space probes are compared with the parameters of the hard (E sub x approximately 55 keV) and thermal X-ray bursts. The electron flux amplitude has been found to correlate with flare importance in the thermal X-ray range (r approximately 0.8). The following two types of flare events have been found in the electron component of SCR. The electron flux increase is accompanied by a hard X-ray burst and the electron spectrum index in the approximately 25 to 200 keV energy range is gamma approximately 2 to 3. The electron flux increase is not accompanied by a hard X-ray burst and the electron spectrum is softer (Delta gamma approximately 0.7 to 1.0).

  17. On the properties of synchrotron-like X-ray emission from laser wakefield accelerated electron beams

    NASA Astrophysics Data System (ADS)

    McGuffey, C.; Schumaker, W.; Matsuoka, T.; Chvykov, V.; Dollar, F.; Kalintchenko, G.; Kneip, S.; Najmudin, Z.; Mangles, S. P. D.; Vargas, M.; Yanovsky, V.; Maksimchuk, A.; Thomas, A. G. R.; Krushelnick, K.

    2018-04-01

    The electric and magnetic fields responsible for electron acceleration in a Laser Wakefield Accelerator (LWFA) also cause electrons to radiate x-ray photons. Such x-ray pulses have several desirable properties including short duration and being well collimated with tunable high energy. We measure the scaling of this x-ray source experimentally up to laser powers greater than 100 TW. An increase in laser power allows electron trapping at a lower density as well as with an increased trapped charge. These effects resulted in an x-ray fluence that was measured to increase non-linearly with laser power. The fluence of x-rays was also compared with that produced from K-α emission resulting from a solid target interaction for the same energy laser pulse. The flux was shown to be comparable, but the LWFA x-rays had a significantly smaller source size. This indicates that such a source may be useful as a backlighter for probing high energy density plasmas with ultrafast temporal resolution.

  18. THE X-RAY DETECTABILITY OF ELECTRON BEAMS ESCAPING FROM THE SUN

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

    Saint-Hilaire, Pascal; Krucker, Saem; Christe, Steven

    2009-05-01

    We study the detectability and characterization of electron beams as they leave their acceleration site in the low corona toward interplanetary space through their nonthermal X-ray bremsstrahlung emission. We demonstrate that the largest interplanetary electron beams ({approx}>10{sup 35} electrons above 10 keV) can be detected in X-rays with current and future instrumentation, such as RHESSI or the X-Ray Telescope (XRT) onboard Hinode. We make a list of optimal observing conditions and beam characteristics. Amongst others, good imaging (as opposed to mere localization or detection in spatially integrated data) is required for proper characterization, putting the requirement on the number ofmore » escaping electrons (above 10 keV) to {approx}>3 x 10{sup 36} for RHESSI, {approx}>3 x 10{sup 35} for Hinode/XRT, and {approx}>10{sup 33} electrons for the FOXSI sounding rocket scheduled to fly in 2011. Moreover, we have found that simple modeling hints at the possibility that coronal soft X-ray jets could be the result of local heating by propagating electron beams.« less

  19. Arsenic microdistribution and speciation in toenail clippings of children living in a historic gold mining area

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

    Pearce, Dora C.; Dowling, Kim; Gerson, Andrea R.

    2010-05-04

    Arsenic is naturally associated with gold mineralization and elevated in some soils and mine waste around historical gold mining activity in Victoria, Australia. To explore uptake, arsenic concentrations in children's toenail clippings and household soils were measured, and the microdistribution and speciation of arsenic in situ in toenail clipping thin sections investigated using synchrotron-based X-ray microprobe techniques. The ability to differentiate exogenous arsenic was explored by investigating surface contamination on cleaned clippings using depth profiling, and direct diffusion of arsenic into incubated clippings. Total arsenic concentrations ranged from 0.15 to 2.1 {micro}g/g (n = 29) in clipping samples and frommore » 3.3 to 130 {micro}g/g (n = 22) in household soils, with significant correlation between transformed arsenic concentrations (Pearson's r = 0.42, P = 0.023) when household soil was treated as independent. In clipping thin sections (n = 2), X-ray fluorescence (XRF) mapping showed discrete layering of arsenic consistent with nail structure, and irregular arsenic incorporation along the nail growth axis. Arsenic concentrations were heterogeneous at 10 x 10 {micro}m microprobe spot locations investigated (< 0.1 to 13.3 {micro}g/g). X-ray absorption near-edge structure (XANES) spectra suggested the presence of two distinct arsenic species: a lower oxidation state species, possibly with mixed sulphur and methyl coordination (denoted As{sub (-S, -ch3)}{sup {approx}III}); and a higher oxidation state species (denoted As{sub (-O)}{sup {approx}V}). Depth profiling suggested that surface contamination was unlikely (n = 4), and XRF and XANES analyses of thin sections of clippings incubated in dry or wet mine waste, or untreated, suggested direct diffusion of arsenic occurred under moist conditions. These findings suggest that arsenic in soil contributes to some systemic absorption associated with periodic exposures among children resident in areas of historic gold mining activity in Victoria, Australia. Future studies are required to ascertain if adverse health effects are associated with current levels of arsenic uptake.« less

  20. A Seafloor Microbial Biome Hosted within Incipient Ferromanganese Crusts

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

    Templeton, Alexis S.; Knowles, A. S.; Eldridge, D. L.

    2009-11-15

    Unsedimented volcanic rocks exposed on the seafloor at ridge systems and Seamounts host complex, abundant and diverse microbial communities that are relatively cosmopolitan in distribution (Lysnes, Thorseth et al. 2004; Mason, Stingl et al. 2007; Santelli, Orcutt et al. 2008). The most commonly held hypothesis is that the energy released by the hydration, dissolution and oxidative alteration of volcanic glasses in seawater drives the formation of an ocean crust biosphere (Thorseth, Furnes et al. 1992; Fisk, Giovannoni et al. 1998; Furnes and Staudigel 1999). The combined thermodynamically favorable weathering reactions could theoretically support anywhere from 105 to 109 cells/gram ofmore » rock depending upon the metabolisms utilized and cellular growth rates and turnover (Bach and Edwards 2003; Santelli, Orcutt et al. 2008). Yet microbially-mediated basalt alteration and energy conservation has not been directly demonstrated on the seafloor. By using synchrotron-based x-ray microprobe mapping, x-ray absorption spectroscopy and high-resolution scanning and transmission electron microscopy observations of young volcanic glasses recovered from the outer flanks of Loihi Seamount, we intended to identify the initial rates and mechanisms of microbial basalt colonization and bioalteration. Instead, here we show that microbial biofilms are intimately associated with ferromanganese crusts precipitating onto basalt surfaces from cold seawater. Thus we hypothesize that microbial communities colonizing seafloor rocks are established and sustained by external inputs of potential energy sources, such as dissolved and particulate Fe(II), Mn(II) and organic matter, rather than rock dissolution.« less

  1. X-ray analysis of electron Bernstein wave heating in MST

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

    Seltzman, A. H., E-mail: seltzman@wisc.edu; Anderson, J. K.; DuBois, A. M.

    2016-11-15

    A pulse height analyzing x-ray tomography system has been developed to detect x-rays from electron Bernstein wave heated electrons in the Madison symmetric torus reversed field pinch (RFP). Cadmium zinc telluride detectors are arranged in a parallel beam array with two orthogonal multi-chord detectors that may be used for tomography. In addition a repositionable 16 channel fan beam camera with a 55° field of view is used to augment data collected with the Hard X-ray array. The chord integrated signals identify target emission from RF heated electrons striking a limiter located 12° toroidally away from the RF injection port. Thismore » provides information on heated electron spectrum, transport, and diffusion. RF induced x-ray emission from absorption on harmonic electron cyclotron resonances in low current (<250 kA) RFP discharges has been observed.« less

  2. Quantitative electron density characterization of soft tissue substitute plastic materials using grating-based x-ray phase-contrast imaging

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

    Sarapata, A.; Chabior, M.; Zanette, I.

    2014-10-15

    Many scientific research areas rely on accurate electron density characterization of various materials. For instance in X-ray optics and radiation therapy, there is a need for a fast and reliable technique to quantitatively characterize samples for electron density. We present how a precise measurement of electron density can be performed using an X-ray phase-contrast grating interferometer in a radiographic mode of a homogenous sample in a controlled geometry. A batch of various plastic materials was characterized quantitatively and compared with calculated results. We found that the measured electron densities closely match theoretical values. The technique yields comparable results between amore » monochromatic and a polychromatic X-ray source. Measured electron densities can be further used to design dedicated X-ray phase contrast phantoms and the additional information on small angle scattering should be taken into account in order to exclude unsuitable materials.« less

  3. High flux femtosecond x-ray emission from the electron-hose instability in laser wakefield accelerators

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

    Dong, C. F.; Zhao, T. Z.; Behm, K.

    Here, bright and ultrashort duration x-ray pulses can be produced by through betatron oscillations of electrons during laser wakefield acceleration (LWFA). Our experimental measurements using the Hercules laser system demonstrate a dramatic increase in x-ray flux for interaction distances beyond the depletion/dephasing lengths, where the initial electron bunch injected into the first wake bucket catches up with the laser pulse front and the laser pulse depletes. A transition from an LWFA regime to a beam-driven plasma wakefield acceleration regime consequently occurs. The drive electron bunch is susceptible to the electron-hose instability and rapidly develops large amplitude oscillations in its tail,more » which leads to greatly enhanced x-ray radiation emission. We measure the x-ray flux as a function of acceleration length using a variable length gas cell. 3D particle-in-cell simulations using a Monte Carlo synchrotron x-ray emission algorithm elucidate the time-dependent variations in the radiation emission processes.« less

  4. High flux femtosecond x-ray emission from the electron-hose instability in laser wakefield accelerators

    NASA Astrophysics Data System (ADS)

    Dong, C. F.; Zhao, T. Z.; Behm, K.; Cummings, P. G.; Nees, J.; Maksimchuk, A.; Yanovsky, V.; Krushelnick, K.; Thomas, A. G. R.

    2018-04-01

    Bright and ultrashort duration x-ray pulses can be produced by through betatron oscillations of electrons during laser wakefield acceleration (LWFA). Our experimental measurements using the Hercules laser system demonstrate a dramatic increase in x-ray flux for interaction distances beyond the depletion/dephasing lengths, where the initial electron bunch injected into the first wake bucket catches up with the laser pulse front and the laser pulse depletes. A transition from an LWFA regime to a beam-driven plasma wakefield acceleration regime consequently occurs. The drive electron bunch is susceptible to the electron-hose instability and rapidly develops large amplitude oscillations in its tail, which leads to greatly enhanced x-ray radiation emission. We measure the x-ray flux as a function of acceleration length using a variable length gas cell. 3D particle-in-cell simulations using a Monte Carlo synchrotron x-ray emission algorithm elucidate the time-dependent variations in the radiation emission processes.

  5. High flux femtosecond x-ray emission from the electron-hose instability in laser wakefield accelerators

    DOE PAGES

    Dong, C. F.; Zhao, T. Z.; Behm, K.; ...

    2018-04-24

    Here, bright and ultrashort duration x-ray pulses can be produced by through betatron oscillations of electrons during laser wakefield acceleration (LWFA). Our experimental measurements using the Hercules laser system demonstrate a dramatic increase in x-ray flux for interaction distances beyond the depletion/dephasing lengths, where the initial electron bunch injected into the first wake bucket catches up with the laser pulse front and the laser pulse depletes. A transition from an LWFA regime to a beam-driven plasma wakefield acceleration regime consequently occurs. The drive electron bunch is susceptible to the electron-hose instability and rapidly develops large amplitude oscillations in its tail,more » which leads to greatly enhanced x-ray radiation emission. We measure the x-ray flux as a function of acceleration length using a variable length gas cell. 3D particle-in-cell simulations using a Monte Carlo synchrotron x-ray emission algorithm elucidate the time-dependent variations in the radiation emission processes.« less

  6. Probing solid catalysts under operating conditions: electrons or X-rays?

    PubMed

    Thomas, John Meurig; Hernandez-Garrido, Juan-Carlos

    2009-01-01

    Seeing is believing: In light of recent advances, the pros and cons of using electrons and X-rays for in situ studies of catalysts are analyzed: by using X-rays the structure of bound reactants at steady state are obtained from extended X-ray adsorption fine structure spectroscopy (EXAFS) data (see graph), thereby affording mechanistic insights.

  7. Quantum theory for 1D X-ray free electron laser

    DOE PAGES

    Anisimov, Petr Mikhaylovich

    2017-09-19

    Classical 1D X-ray Free Electron Laser (X-ray FEL) theory has stood the test of time by guiding FEL design and development prior to any full-scale analysis. Future X-ray FELs and inverse-Compton sources, where photon recoil approaches an electron energy spread value, push the classical theory to its limits of applicability. After substantial efforts by the community to find what those limits are, there is no universally agreed upon quantum approach to design and development of future X-ray sources. We offer a new approach to formulate the quantum theory for 1D X-ray FELs that has an obvious connection to the classicalmore » theory, which allows for immediate transfer of knowledge between the two regimes. In conclusion, we exploit this connection in order to draw quantum mechanical conclusions about the quantum nature of electrons and generated radiation in terms of FEL variables.« less

  8. Quantum theory for 1D X-ray free electron laser

    NASA Astrophysics Data System (ADS)

    Anisimov, Petr M.

    2018-06-01

    Classical 1D X-ray Free Electron Laser (X-ray FEL) theory has stood the test of time by guiding FEL design and development prior to any full-scale analysis. Future X-ray FELs and inverse-Compton sources, where photon recoil approaches an electron energy spread value, push the classical theory to its limits of applicability. After substantial efforts by the community to find what those limits are, there is no universally agreed upon quantum approach to design and development of future X-ray sources. We offer a new approach to formulate the quantum theory for 1D X-ray FELs that has an obvious connection to the classical theory, which allows for immediate transfer of knowledge between the two regimes. We exploit this connection in order to draw quantum mechanical conclusions about the quantum nature of electrons and generated radiation in terms of FEL variables.

  9. X-ray diagnostic development for measurement of electron deposition to the SABRE anode

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

    Lash, J.S.; Derzon, M.S.; Cuneo, M.E.

    Extraction applied-B ion diodes are under development on the SABRE (6 MV, 250 kA) accelerator at Sandia. The authors are assessing this technology for the production of high brightness lithium ion beams for inertial confinement fusion. Electron loss physics is a focus of effort since electron sheath physics affects ion beam divergence, ion beam purity, and diode impedance. An x-ray slit-imaging diagnostic is under development for detection of x-rays produced during electron deposition to the anode. This diagnostic will aid in the correlation of electron deposition to ion production to better understand the ion diode physics. The x-ray detector consistsmore » of a filter pack, scintillator and optical fiber array that is streaked onto a CCD camera. Current orientation of the diagnostic provides spatial information across the anode radius at three different azimuths or at three different x-ray energy cuts. The observed x-ray emission spectrum can then be compared to current modeling efforts examining electron deposition to the anode.« less

  10. Radiation of X-Rays Using Uniaxially Polarized LiNbO3 Single Crystal

    NASA Astrophysics Data System (ADS)

    Fukao, Shinji; Nakanishi, Yoshikazu; Mizoguchi, Tadahiro; Ito, Yoshiaki; Nakamura, Toru; Yoshikado, Shinzo

    2009-03-01

    X-rays are radiated due to the bremsstrahlung caused by the collision of electrons with a metal target placed opposite the negative electric surface of a crystal by changing the temperature of a LiNbO3 single crystal uniaxially polarized in the c-axis direction. It is suggested that both electric field intensity and electron density determine the intensity of X-ray radiation. Electrons are supplied by the ionization of residual gas in space, field emission from a case inside which a crystal is located, considered to be due to the high electric-field intensity formed by the surface charges on the crystal, and an external electron source, such as a thermionic source. In a high vacuum, it was found that the electrons supplied by electric-field emission mainly contribute to the radiation of X-rays. It was found that the integrated intensity of X-rays can be maximized by supplying electrons both external and by electric-field emission. Furthermore, the integrated intensity of the X-rays is stable for many repeated temperature changes.

  11. On the modulation of X ray fluxes in thunderstorms

    NASA Technical Reports Server (NTRS)

    Mccarthy, Michael P.; Parks, George K.

    1992-01-01

    The production of X-ray fluxes in thunderstorms has been attributed to bremsstrahlung. Assuming this, another question arises. How can a thunderstorm modulate the number density of electrons which are sufficiently energetic to produce X-rays? As a partial answer to this question, the effects of typical thunderstorm electric fields on a background population of energetic electrons, such as produced by cosmic ray secondaries and their decays or the decay of airborne radionuclides, are considered. The observed variation of X-ray flux is shown to be accounted for by a simple model involving typical electric field strengths. A necessary background electron number density is found from the model and is determined to be more than 2 orders of magnitude higher than that available from radon decay and a factor of 8 higher than that available from cosmic ray secondaries. The ionization enhancement due to energetic electrons and X-rays is discussed.

  12. Femtosecond all-optical synchronization of an X-ray free-electron laser

    DOE PAGES

    Schulz, S.; Grguraš, I.; Behrens, C.; ...

    2015-01-20

    Many advanced applications of X-ray free-electron lasers require pulse durations and time resolutions of only a few femtoseconds. To generate these pulses and to apply them in time-resolved experiments, synchronization techniques that can simultaneously lock all independent components, including all accelerator modules and all external optical lasers, to better than the delivered free-electron laser pulse duration, are needed. Here we achieve all-optical synchronization at the soft X-ray free-electron laser FLASH and demonstrate facility-wide timing to better than 30 fs r.m.s. for 90 fs X-ray photon pulses. Crucially, our analysis indicates that the performance of this optical synchronization is limited primarilymore » by the free-electron laser pulse duration, and should naturally scale to the sub-10 femtosecond level with shorter X-ray pulses.« less

  13. Time-dependent Schrödinger equation for molecular core-hole dynamics

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

    Picón, A.

    2017-02-01

    X-ray spectroscopy is an important tool for the investigation of matter. X rays primarily interact with inner-shell electrons, creating core (inner-shell) holes that will decay on the time scale of attoseconds to a few femtoseconds through electron relaxations involving the emission of a photon or an electron. Furthermore, the advent of femtosecond x-ray pulses expands x-ray spectroscopy to the time domain and will eventually allow the control of core-hole population on time scales comparable to core-vacancy lifetimes. For both cases, a theoretical approach that accounts for the x-ray interaction while the electron relaxations occur is required. We describe a time-dependentmore » framework, based on solving the time-dependent Schrödinger equation, that is suitable for describing the induced electron and nuclear dynamics.« less

  14. Femtosecond all-optical synchronization of an X-ray free-electron laser

    PubMed Central

    Schulz, S.; Grguraš, I.; Behrens, C.; Bromberger, H.; Costello, J. T.; Czwalinna, M. K.; Felber, M.; Hoffmann, M. C.; Ilchen, M.; Liu, H. Y.; Mazza, T.; Meyer, M.; Pfeiffer, S.; Prędki, P.; Schefer, S.; Schmidt, C.; Wegner, U.; Schlarb, H.; Cavalieri, A. L.

    2015-01-01

    Many advanced applications of X-ray free-electron lasers require pulse durations and time resolutions of only a few femtoseconds. To generate these pulses and to apply them in time-resolved experiments, synchronization techniques that can simultaneously lock all independent components, including all accelerator modules and all external optical lasers, to better than the delivered free-electron laser pulse duration, are needed. Here we achieve all-optical synchronization at the soft X-ray free-electron laser FLASH and demonstrate facility-wide timing to better than 30 fs r.m.s. for 90 fs X-ray photon pulses. Crucially, our analysis indicates that the performance of this optical synchronization is limited primarily by the free-electron laser pulse duration, and should naturally scale to the sub-10 femtosecond level with shorter X-ray pulses. PMID:25600823

  15. Mapping Metal Elements of Shuangbai Dinosaur Fossil by Synchrotron X-ray Fluorescence Microprobe

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

    Wang, Y.; Qun, Y; Ablett, J

    The metal elements mapping of Shuangbai dinosaur fossil, was obtained by synchrotron x-ray fluorescence (SXRF). Eight elements, Ca, Mn, Fe, Cu, Zn, As, Y and Sr were determined. Elements As and Y were detected for the first time in the dinosaur fossil. The data indicated that metal elements are asymmetrical on fossil section. This is different from common minerals. Mapping metals showed that metal element As is few. The dinosaur most likely belongs to natural death. This is different from Zigong dinosaurs which were found dead from poisoning. This method has been used to find that metals Fe and Mnmore » are accrete, and the same is true for Sr and Y. This study indicated that colloid granule Fe and Mn, as well as Sr and Y had opposite electric charges in lithification process of fossils. By this analysis, compound forms can be ascertained. Synchrotron light source x-ray fluorescence is a complementary method that shows mapping of metal elements at the dinosaur fossil, and is rapid, exact and intuitionist. This study shows that dinosaur fossil mineral imaging has a potential in reconstructing the paleoenvironment and ancient geology.« less

  16. X-ray Absorption Near Edge Structure Spectroscopy to Resolve the in Vivo Chemistry of the Redox-Active Indazolium trans-[Tetrachlorobis(1H-indazole)ruthenate(III)] (KP1019)

    PubMed Central

    2013-01-01

    Indazolium trans-[tetrachlorobis(1H-indazole)ruthenate(III)] (1, KP1019) and its analogue sodium trans-[tetrachlorobis(1H-indazole)ruthenate(III)] (2, KP1339) are promising redox-active anticancer drug candidates that were investigated with X-ray absorption near edge structure spectroscopy. The analysis was based on the concept of the coordination charge and ruthenium model compounds representing possible coordinations and oxidation states in vivo. 1 was investigated in citrate saline buffer (pH 3.5) and in carbonate buffer (pH 7.4) at 37 °C for different time intervals. Interaction studies on 1 with glutathione in saline buffer and apo-transferrin in carbonate buffer were undertaken, and the coordination of 1 and 2 in tumor tissues was studied too. The most likely coordinations and oxidation states of the compound under the above mentioned conditions were assigned. Microprobe X-ray fluorescence of tumor thin sections showed the strong penetration of ruthenium into the tumor tissue, with the highest concentrations near blood vessels and in the edge regions of the tissue samples. PMID:23282017

  17. Do selenium hyperaccumulators affect selenium speciation in neighboring plants and soil? An X-Ray Microprobe Analysis.

    PubMed

    El Mehdawi, Ali F; Lindblom, Stormy D; Cappa, Jennifer J; Fakra, Sirine C; Pilon-Smits, Elizabeth A H

    2015-01-01

    Neighbors of Se hyperaccumulators Stanleya pinnata and Astragalus bisulcatus were found earlier to have elevated Se levels. Here we investigate whether Se hyperaccumulators affect Se localization and speciation in surrounding soil and neighboring plants. X-ray fluorescence mapping and X-ray absorption near-edge structure spectroscopy were used to analyze Se localization and speciation in leaves of Artemisia ludoviciana, Symphyotrichum ericoides and Chenopodium album growing next to Se hyperaccumulators or non-accumulators at a seleniferous site. Regardless of neighbors, A. ludoviciana, S. ericoides and C. album accumulated predominantly (73-92%) reduced selenocompounds with XANES spectra similar to the C-Se-C compounds selenomethionine and methyl-selenocysteine. Preliminary data indicate that the largest Se fraction (65-75%), both in soil next to hyperaccumulator S. pinnata and next to nonaccumulator species was reduced Se with spectra similar to C-Se-C standards. These same C-Se-C forms are found in hyperaccumulators. Thus, hyperaccumulator litter may be a source of organic soil Se, but soil microorganisms may also contribute. These findings are relevant for phytoremediation and biofortification since organic Se is more readily accumulated by plants, and more effective for dietary Se supplementation.

  18. 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.

  19. Using DTSA-II to simulate and interpret energy dispersive spectra from particles.

    PubMed

    Ritchie, Nicholas W M

    2010-06-01

    A high quality X-ray spectrum image of a 3.3 mum diameter sphere of K411 glass resting on a copper substrate was collected at 25 keV. The same sample configuration was modeled using the NISTMonte Monte Carlo simulation of electron and X-ray transport as is integrated into the quantitative X-ray microanalysis software package DTSA-II. The distribution of measured and simulated X-ray intensity compare favorably for all the major lines present in the spectra. The simulation is further examined to investigate the influence of angle-of-incidence, sample thickness, and sample diameter on the generated and measured X-ray intensity. The distribution of generated X-rays is seen to deviate significantly from a naive model which assumes that the distribution of generated X-rays is similar to bulk within the volume they share in common. It is demonstrated that the angle at which the electron beam strikes the sample has nonnegligible consequences. It is also demonstrated that within the volume that the bulk and particle share in common that electrons, which have exited and later reentered the particle volume, generate a significant fraction of the X-rays. Any general model of X-ray generation in particles must take into account the lateral spread of the scattered electron beam.

  20. Core Community Specifications for Electron Microprobe Operating Systems: Software, Quality Control, and Data Management Issues

    NASA Technical Reports Server (NTRS)

    Fournelle, John; Carpenter, Paul

    2006-01-01

    Modem electron microprobe systems have become increasingly sophisticated. These systems utilize either UNIX or PC computer systems for measurement, automation, and data reduction. These systems have undergone major improvements in processing, storage, display, and communications, due to increased capabilities of hardware and software. Instrument specifications are typically utilized at the time of purchase and concentrate on hardware performance. The microanalysis community includes analysts, researchers, software developers, and manufacturers, who could benefit from exchange of ideas and the ultimate development of core community specifications (CCS) for hardware and software components of microprobe instrumentation and operating systems.

  1. Determination of trace element mineral/liquid partition coefficients in melilite and diopside by ion and electron microprobe techniques

    NASA Technical Reports Server (NTRS)

    Kuehner, S. M.; Laughlin, J. R.; Grossman, L.; Johnson, M. L.; Burnett, D. S.

    1989-01-01

    The applicability of ion microprobe (IMP) for quantitative analysis of minor elements (Sr, Y, Zr, La, Sm, and Yb) in the major phases present in natural Ca-, Al-rich inclusions (CAIs) was investigated by comparing IMP results with those of an electron microprobe (EMP). Results on three trace-element-doped glasses indicated that it is not possible to obtain precise quantitative analysis by using IMP if there are large differences in SiO2 content between the standards used to derive the ion yields and the unknowns.

  2. Two-colour hard X-ray free-electron laser with wide tunability.

    PubMed

    Hara, Toru; Inubushi, Yuichi; Katayama, Tetsuo; Sato, Takahiro; Tanaka, Hitoshi; Tanaka, Takashi; Togashi, Tadashi; Togawa, Kazuaki; Tono, Kensuke; Yabashi, Makina; Ishikawa, Tetsuya

    2013-01-01

    Ultrabrilliant, femtosecond X-ray pulses from X-ray free-electron lasers (XFELs) have promoted the investigation of exotic interactions between intense X-rays and matters, and the observation of minute targets with high spatio-temporal resolution. Although a single X-ray beam has been utilized for these experiments, the use of multiple beams with flexible and optimum beam parameters should drastically enhance the capability and potentiality of XFELs. Here we show a new light source of a two-colour double-pulse (TCDP) XFEL in hard X-rays using variable-gap undulators, which realizes a large and flexible wavelength separation of more than 30% with an ultraprecisely controlled time interval in the attosecond regime. Together with sub-10-fs pulse duration and multi-gigawatt peak powers, the TCDP scheme enables us to elucidate X-ray-induced ultrafast transitions of electronic states and structures, which will significantly contribute to the advancement of ultrafast chemistry, plasma and astronomical physics, and quantum X-ray optics.

  3. Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

    PubMed

    Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

    2014-05-02

    Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge.

  4. The X-ray Detectability of Electron Beams Escaping from the Sun

    NASA Astrophysics Data System (ADS)

    Saint-Hilaire, Pascal; Krucker, Säm; Christe, Steven; Lin, Robert P.

    2009-05-01

    We study the detectability and characterization of electron beams as they leave their acceleration site in the low corona toward interplanetary space through their nonthermal X-ray bremsstrahlung emission. We demonstrate that the largest interplanetary electron beams (gsim1035 electrons above 10 keV) can be detected in X-rays with current and future instrumentation, such as RHESSI or the X-Ray Telescope (XRT) onboard Hinode. We make a list of optimal observing conditions and beam characteristics. Amongst others, good imaging (as opposed to mere localization or detection in spatially integrated data) is required for proper characterization, putting the requirement on the number of escaping electrons (above 10 keV) to gsim3 × 1036 for RHESSI, gsim3 × 1035 for Hinode/XRT, and gsim1033 electrons for the FOXSI sounding rocket scheduled to fly in 2011. Moreover, we have found that simple modeling hints at the possibility that coronal soft X-ray jets could be the result of local heating by propagating electron beams.

  5. Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

    NASA Astrophysics Data System (ADS)

    Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

    2014-04-01

    The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called ``molecular movie'' within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.

  6. Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

    PubMed Central

    Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

    2014-01-01

    The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes. PMID:24740172

  7. Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

    DOE PAGES

    Gaudin, J.; Fourment, C.; Cho, B. I.; ...

    2014-04-17

    The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level ofmore » the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.« less

  8. Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

    DOE PAGES

    Tilka, J. A.; Park, J.; Ahn, Y.; ...

    2016-07-06

    Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

  9. Strain-dependent evolution of garnets in a high pressure ductile shear zone using Synchroton x-ray microtomography

    NASA Astrophysics Data System (ADS)

    Macente, Alice; Fusseis, Florian; Menegon, Luca; John, Timm

    2016-04-01

    Synkinematic reaction microfabrics carry important information on the kinetics, timing and rheology of tectonometamorphic processes. Despite being routinely interpreted in metamorphic and structural studies, reaction and deformation microfabrics are usually described in two dimensions. We applied Synchrotron-based x-ray microtomography to document the evolution of a pristine olivine gabbro into a deformed omphacite-garnet eclogite in 3D. In the investigated samples, which cover a strain gradient into a shear zone from the Western Gneiss Region (Norway) previously described by John et al., (2009), we focused on the spatial transformation of garnet coronas into elongated clusters of garnets. Our microtomographic data allowed us to quantify changes to the garnet volume, their shapes and their spatial arrangement. We combined microtomographic observations with light microscope- and backscatter electron images as well as electron microprobe- (EMPA) and electron backscatter diffraction (EBSD) analyses to correlate mineral composition and orientation data with the x-ray absorption signal of the same mineral grains. This allowed us to extrapolate our interpretation of the metamorphic microfabric evolution to the third dimension, effectively yielding a 4-dimensional dataset. We found that: - The x-ray absorption contrast between individual mineral phases in our microtomographic data is sufficient to allow the same petrographic observations than in light- and electron microscopy, but extended to 3D. - Amongst the major constituents of the synkinematic reactions, garnet is the only phase that can be segmented confidently from the microtomographic data. - With increasing deformation, the garnet volume increases from about 9% to 25%. - Garnet coronas in the gabbros never completely encapsulate olivine grains. This may indicate that the reaction progressed preferentially in some directions, but also leaves pathways for element transport to and from the olivines that are unobstructed by reaction products. - Neighbouring garnet coronas are interconnected, i.e. in direct contact to each other. From a mechanical point of view, we interpret touching garnet coronas that form a rigid, potentially load-supporting framework to affect the rheology of the rock. - In the most highly deformed eclogites, the oblate shapes of elongated garnet clusters reflect a deformational origin of the microfabrics. The clusters define a foliation, whose orientation and intensity we quantified using a star volume distribution algorithm. We interpret the aligned garnet clusters to direct synkinematic fluid flow and consequently influence the transport of dissolved chemical components. - EBSD on garnets shows that, there is no evidence for crystal plastic deformation and all the garnets are internally strain free and show a near-random crystal preferred orientation. There is, however evidence for minor fracturing. We interpret these observations as pointing to a mechanical disintegration of the garnet coronas during strain localisation, and their rearrangement into individual clusters. This process will have been supported by pressure solution/reprecipitation processes. Our study clearly demonstrates what 3- or even 4-dimensional data from reaction microfabrics can add to the understanding of metamorphic processes.

  10. Elastic Wave Velocity Measurements on Mantle Peridotite at High Pressure and Temperature

    NASA Astrophysics Data System (ADS)

    Mistler, G. W.; Ishikawa, M.; Li, B.

    2002-12-01

    With the success of conducting ultrasonic measurements at high pressure and high temperature in large volume high pressure apparatus with in-situ measurement of the sample length by X-ray imaging, it is now possible to measure elastic wave velocities on aggregate samples with candidate compositions of the mantle to the conditions of the Earth's transition zone in the laboratory. These data can be directly compared with seismic data to distinguish the compositional models in debate. In this work, we carried out velocity measurements on natural peridotite KLB-1 at the conditions of the Earth's upper mantle. Fine powered sample of natural KLB-1 was used as starting material. Specimens for ultrasonic measurements were hot-pressed and equilibrated at various pressure and temperature conditions along geotherm up to the transition zone. The recovered samples were characterized with density measurement, X-ray diffraction and microprobe analysis. Bench top P and S wave velocities of KLB-1 sample sintered at 3-4 GPa and 1400 degree centigrade showed a very good agreement with the VRH average of pyrolite. High pressure and high temperature measurements was conducted up to 7 GPa and 800 degree centigrade using ultrasonic interferometric method in a DIA-type high pressure apparatus in conjunction with X-ray diffraction and X-ray imaging. The utilization of X-ray imaging technique provides direct measurements of sample lengths at high pressure and high temperature, ensuring a precise determination of velocities. The results of P and S wave velocities at high pressure and high temperature as well as their comparison with calculated pyrolite model will be presented.

  11. Determination of nitrogen in coal macerals using electron microprobe technique-experimental procedure

    USGS Publications Warehouse

    Mastalerz, Maria; Gurba, L.W.

    2001-01-01

    This paper discusses nitrogen determination with the Cameca SX50 electron microprobe using PCO as an analyzing crystal. A set of conditions using differing accelerating voltages, beam currents, beam sizes, and counting times were tested to determine parameters that would give the most reliable nitrogen determination. The results suggest that, for the instrumentation used, 10 kV, current 20 nA, and a counting time of 20 s provides the most reliable nitrogen determination, with a much lower detection limit than the typical concentration of this element in coal. The study demonstrates that the electron microprobe technique can be used to determine the nitrogen content of coal macerals successfully and accurately. ?? 2001 Elsevier Science B.V. All rights reserved.

  12. Diffusive transport of energetic electrons in the solar corona: X-ray and radio diagnostics

    NASA Astrophysics Data System (ADS)

    Musset, S.; Kontar, E. P.; Vilmer, N.

    2018-02-01

    Context. Imaging spectroscopy in X-rays with RHESSI provides the possibility to investigate the spatial evolution of X-ray emitting electron distribution and therefore, to study transport effects on energetic electrons during solar flares. Aims: We study the energy dependence of the scattering mean free path of energetic electrons in the solar corona. Methods: We used imaging spectroscopy with RHESSI to study the evolution of energetic electrons distribution in various parts of the magnetic loop during the 2004 May 21 flare. We compared these observations with the radio observations of the gyrosynchrotron radiation of the same flare and with the predictions of a diffusive transport model. Results: X-ray analysis shows a trapping of energetic electrons in the corona and a spectral hardening of the energetic electron distribution between the top of the loop and the footpoints. Coronal trapping of electrons is stronger for radio-emitting electrons than for X-ray-emitting electrons. These observations can be explained by a diffusive transport model. Conclusions: We show that the combination of X-ray and radio diagnostics is a powerful tool to study electron transport in the solar corona in different energy domains. We show that the diffusive transport model can explain our observations, and in the range 25-500 keV, the scattering mean free path of electrons decreases with electron energy. We can estimate for the first time the scattering mean free path dependence on energy in the corona.

  13. Liquid sample delivery techniques for serial femtosecond crystallography

    PubMed Central

    Weierstall, Uwe

    2014-01-01

    X-ray free-electron lasers overcome the problem of radiation damage in protein crystallography and allow structure determination from micro- and nanocrystals at room temperature. To ensure that consecutive X-ray pulses do not probe previously exposed crystals, the sample needs to be replaced with the X-ray repetition rate, which ranges from 120 Hz at warm linac-based free-electron lasers to 1 MHz at superconducting linacs. Liquid injectors are therefore an essential part of a serial femtosecond crystallography experiment at an X-ray free-electron laser. Here, we compare different techniques of injecting microcrystals in solution into the pulsed X-ray beam in vacuum. Sample waste due to mismatch of the liquid flow rate to the X-ray repetition rate can be addressed through various techniques. PMID:24914163

  14. 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.

  15. Energetic electrons, hard x-ray emission and MHD activity studies in the IR-T1 tokamak.

    PubMed

    Agah, K Mikaili; Ghoranneviss, M; Elahi, A Salar

    2015-01-01

    Determinations of plasma parameters as well as the Magnetohydrodynamics (MHD) activity, energetic electrons energy and energy confinement time are essential for future fusion reactors experiments and optimized operation. Also some of the plasma information can be deduced from these parameters, such as plasma equilibrium, stability, and MHD instabilities. In this contribution we investigated the relation between energetic electrons, hard x-ray emission and MHD activity in the IR-T1 Tokamak. For this purpose we used the magnetic diagnostics and a hard x-ray spectroscopy in IR-T1 tokamak. A hard x-ray emission is produced by collision of the runaway electrons with the plasma particles or limiters. The mean energy was calculated from the slope of the energy spectrum of hard x-ray photons.

  16. Systematic design and three-dimensional simulation of X-ray FEL oscillator for Shanghai Coherent Light Facility

    NASA Astrophysics Data System (ADS)

    Li, Kai; Deng, Haixiao

    2018-07-01

    The Shanghai Coherent Light Facility (SCLF) is a quasi-continuous wave hard X-ray free electron laser facility, which is currently under construction. Due to the high repetition rate and high-quality electron beams, it is straightforward to consider X-ray free electron laser oscillator (XFELO) operation for the SCLF. In this paper, the main processes for XFELO design, and parameter optimization of the undulator, X-ray cavity, and electron beam are described. A three-dimensional X-ray crystal Bragg diffraction code, named BRIGHT, was introduced for the first time, which can be combined with the GENESIS and OPC codes for the numerical simulations of the XFELO. The performance of the XFELO of the SCLF is investigated and optimized by theoretical analysis and numerical simulation.

  17. Development of a simulation method for dynamics of electrons ejected from DNA molecules irradiated with X-rays.

    PubMed

    Kai, Takeshi; Higuchi, Mariko; Fujii, Kentaro; Watanabe, Ritsuko; Yokoya, Akinari

    2012-12-01

    To develop a method for simulating the dynamics of the photoelectrons and Auger electrons ejected from DNA molecules irradiated with pulsed monochromatic X-rays. A 30-base-pair (bp) DNA molecule was used as the target model, and the X-rays were assumed to have a Gaussian-shaped time distribution. Photoionization and Auger decay were considered as the atomic processes. The atoms from which the photoelectrons or Auger electrons were emitted were specified in the DNA molecule (or DNA ion) using the Monte Carlo method, and the trajectory of each electron in the electric field formed around the positively charged DNA molecule was calculated with a Newtonian equation. The kinetics of the electrons produced by irradiation with X-rays at an intensity ranging from 1 × 10(12) to 1 × 10(16) photons/mm(2) and energies of 380 eV (below the carbon K-edge), 435 eV (above the nitrogen K-edge), and 560 eV (above the oxygen K-edge) were evaluated. It was found that at an X-ray intensity of 1 × 10(14) photons/mm(2) or less, all the produced electrons escaped from the target. However, above an X-ray intensity of 1 × 10(15) photons/mm(2) and an energy of 560 eV, some photoelectrons that were ejected from the oxygen atoms were trapped near the target DNA. A simulation method for studying the trajectories of electrons ejected from a 30-bp DNA molecule irradiated with pulsed monochromatic X-rays has been developed. The present results show that electron dynamics are strongly dependent on the charged density induced in DNA by pulsed X-ray irradiation.

  18. Olivine-melt relationships and syneruptive redox variations in the 1959 eruption of K$$\\bar{i}$$lauea Volcano as revealed by XANES

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

    Helz, R. T.; Cottrell, E.; Brounce, M. N.

    The 1959 summit eruption of Kmore » $$\\bar{i}$$lauea Volcano exhibited high lava fountains of gas-rich, primitive magma, containing olivine + chromian spinel in highly vesicular brown glass. Microprobe analysis of these samples shows that euhedral rims on olivine phenocrysts, in direct contact with glass, vary significantly in forsterite (Fo) content, at constant major-element melt composition, as do unzoned groundmass olivine crystals. Ferric/total iron (Fe+ 3/FeT)ratios for matrix and interstitial glasses, plus olivine-hosted glass inclusions in eight 1959 scoria samples have been determined by micro X-ray absorption near-edge structure spectroscopy (μ-XANES). These data show that much of the variation in Fo content reflects variation in oxidation state of iron in the melt, which varies with sulfur concentration in the glass and (locally) with proximity to scoria edges in contact with air. Data for 24 olivine-melt pairs in the better-equilibrated samples from later in the eruption show KD averaging 0.280 ± 0.03 for the exchange of Fe and Mg between olivine and melt, somewhat displaced from the value of 0.30 ± 0.03 given by Roeder and Emslie (1970). This may reflect the low SiO2 content of the 1959 magmas, which is lower than that in most K$$\\bar{i}$$lauea tholeiites. More broadly, we show the potential of μ-XANES and electron microprobe to revisit and refine the value of KD in natural systems.« less

  19. A vacuum-sealed compact x-ray tube based on focused carbon nanotube field-emission electrons

    NASA Astrophysics Data System (ADS)

    Jeong, Jin-Woo; Kim, Jae-Woo; Kang, Jun-Tae; Choi, Sungyoul; Ahn, Seungjoon; Song, Yoon-Ho

    2013-03-01

    We report on a fully vacuum-sealed compact x-ray tube based on focused carbon nanotube (CNT) field-emission electrons for various radiography applications. The specially designed two-step brazing process enabled us to accomplish a good vacuum level for the stable and reliable operation of the x-ray tube without any active vacuum pump. Also, the integrated focusing electrodes in the field-emission electron gun focused electron beams from the CNT emitters onto the anode target effectively, giving a small focal spot of around 0.3 mm with a large current of above 50 mA. The active-current control through the cathode electrode of the x-ray tube led a fast digital modulation of x-ray dose with a low voltage of below 5 V. The fabricated compact x-ray tube showed a stable and reliable operation, indicating good maintenance of a vacuum level of below 5 × 10-6 Torr and the possibility of field-emission x-ray tubes in a stand-alone device without an active pumping system.

  20. Design and characterization of electron beam focusing for X-ray generation in novel medical imaging architecturea

    PubMed Central

    Bogdan Neculaes, V.; Zou, Yun; Zavodszky, Peter; Inzinna, Louis; Zhang, Xi; Conway, Kenneth; Caiafa, Antonio; Frutschy, Kristopher; Waters, William; De Man, Bruno

    2014-01-01

    A novel electron beam focusing scheme for medical X-ray sources is described in this paper. Most vacuum based medical X-ray sources today employ a tungsten filament operated in temperature limited regime, with electrostatic focusing tabs for limited range beam optics. This paper presents the electron beam optics designed for the first distributed X-ray source in the world for Computed Tomography (CT) applications. This distributed source includes 32 electron beamlets in a common vacuum chamber, with 32 circular dispenser cathodes operated in space charge limited regime, where the initial circular beam is transformed into an elliptical beam before being collected at the anode. The electron beam optics designed and validated here are at the heart of the first Inverse Geometry CT system, with potential benefits in terms of improved image quality and dramatic X-ray dose reduction for the patient. PMID:24826066

  1. Table-top laser-driven ultrashort electron and X-ray source: the CIBER-X source project

    NASA Astrophysics Data System (ADS)

    Girardeau-Montaut, Jean-Pierre; Kiraly, Bélà; Girardeau-Montaut, Claire; Leboutet, Hubert

    2000-09-01

    We report on the development of a new laser-driven table-top ultrashort electron and X-ray source, also called the CIBER-X source . X-ray pulses are produced by a three-step process which consists of the photoelectron emission from a thin metallic photocathode illuminated by 16 ps duration laser pulses at 213 nm. The e-gun is a standard Pierce diode electrode type, in which electrons are accelerated by a cw electric field of ˜11 MV/m up to a hole made in the anode. The photoinjector produces a train of 70-80 keV electron pulses of ˜0.5 nC and 20 A peak current at a repetition rate of 10 Hz. The electrons are then transported outside the diode along a path of 20 cm length, and are focused onto a target of thullium by magnetic fields produced by two electromagnetic coils. X-rays are then produced by the impact of electrons on the target. Simulations of geometrical, electromagnetic fields and energetic characteristics of the complete source were performed previously with the assistance of the code PIXEL1 also developed at the laboratory. Finally, experimental electron and X-ray performances of the CIBER-X source as well as its application to very low dose imagery are presented and discussed. source Compacte d' Impulsions Brèves d' Electrons et de Rayons X

  2. The gamma-ray emitting region of the jet in Cyg X-3

    NASA Astrophysics Data System (ADS)

    Zdziarski, Andrzej A.; Sikora, Marek; Dubus, Guillaume; Yuan, Feng; Cerutti, Benoit; Ogorzałek, Anna

    2012-04-01

    We study models of the γ-ray emission of Cyg X-3 observed by Fermi. We calculate the average X-ray spectrum during the γ-ray active periods. Then, we calculate spectra from Compton scattering of a photon beam into a given direction by isotropic relativistic electrons with a power-law distribution, both based on the Klein-Nishina cross-section and in the Thomson limit. Applying the results to scattering of stellar blackbody radiation in the inner jet of Cyg X-3, we find that a low-energy break in the electron distribution at a Lorentz factor of ˜300-103 is required by the shape of the observed X-ray/γ-ray spectrum in order to avoid overproducing the observed X-ray flux. The electrons giving rise to the observed γ-rays are efficiently cooled by Compton scattering, and the power-law index of the acceleration process is ≃2.5-3. The bulk Lorentz factor of the jet and the kinetic power before the dissipation region depend on the fraction of the dissipation power supplied to the electrons; if it is ≃1/2, the Lorentz factor is ˜2.5, and the kinetic power is ˜1038 erg s-1, which represents a firm lower limit on the jet power, and is comparable to the bolometric luminosity of Cyg X-3. Most of the power supplied to the electrons is radiated. The broad-band spectrum constrains the synchrotron and self-Compton emission from the γ-ray emitting electrons, which requires the magnetic field to be relatively weak, with the magnetic energy density ≲ a few times 10-3 of that in the electrons. The actual value of the magnetic field strength can be inferred from a future simultaneous measurement of the infrared and γ-ray fluxes.

  3. Resonantly Enhanced Betatron Hard X-rays from Ionization Injected Electrons in a Laser Plasma Accelerator

    PubMed Central

    Huang, K.; Li, Y. F.; Li, D. Z.; Chen, L. M.; Tao, M. Z.; Ma, Y.; Zhao, J. R.; Li, M. H.; Chen, M.; Mirzaie, M.; Hafz, N.; Sokollik, T.; Sheng, Z. M.; Zhang, J.

    2016-01-01

    Ultrafast betatron x-ray emission from electron oscillations in laser wakefield acceleration (LWFA) has been widely investigated as a promising source. Betatron x-rays are usually produced via self-injected electron beams, which are not controllable and are not optimized for x-ray yields. Here, we present a new method for bright hard x-ray emission via ionization injection from the K-shell electrons of nitrogen into the accelerating bucket. A total photon yield of 8 × 108/shot and 108 photons with energy greater than 110 keV is obtained. The yield is 10 times higher than that achieved with self-injection mode in helium under similar laser parameters. The simulation suggests that ionization-injected electrons are quickly accelerated to the driving laser region and are subsequently driven into betatron resonance. The present scheme enables the single-stage betatron radiation from LWFA to be extended to bright γ-ray radiation, which is beyond the capability of 3rd generation synchrotrons. PMID:27273170

  4. Mineralogical, chemical, and crystallographic properties of supergene jarosite-group minerals from the Xitieshan Pb-Zn sulfide deposit, northern Tibetan Plateau, China

    USGS Publications Warehouse

    Chen, Lei; Li, Jian-Wei; Rye, Robert O.; Benzel, William H.; Lowers, H.A.; He, Ming-Zhong

    2013-01-01

    Supergene jarosite-group minerals are widespread in weathering profiles overlying Pb-Zn sulfide ores at Xitieshan, northern Tibetan Plateau, China. They consist predominantly of K-deficient natrojarosite, with lesser amounts of K-rich natrojarosite and plumbojarosite. Electron microprobe (EMP) analyses, scanning electron microcopy (SEM) investigation, and X-ray mapping reveal that the jarosite-group minerals are characterized by spectacular oscillatory zoning composed of alternating growth bands of K-deficient and K-bearing natrojarosite (K2O >1 wt.%). Plumbojarosite, whenever present, occurs as an overgrowth in the outermost bands, and its composition can be best represented by K0.29Na0.19Pb0.31Fe2.66Al0.22(SO4)1.65(PO4)0.31(AsO4)0.04(OH)7.37. The substitution of monovalent for divalent cations at the A site of plumbojarosite is charge balanced by the substitution of five-valent for six-valent anions in XO,4/sub> at the X site. Thermogravimetric analysis (TGA) of representative samples reveal mass losses of 11.46 wt.% at 446.6 °C and 21.42 wt.% at 683.4 °C due to dehydroxylation and desulfidation, respectively. TGA data also indicate that the natrojarosite structure collapses at 446.6 °C, resulting in the formation of NaFe(SO4)2 and minor hematite. The decomposition products of NaFe(SO4) are hematite and Na,2SO4. Powder X-ray diffraction (XRD) analyses show that the jarosite-group minerals have mean unit-cell parameters of a=7.315 ä and c=016.598 ä. XRD and EMP data support the view that substitutions of Na for K in the A site and full Fe occupancy in the B site can considerably decrease the unit-cell parameter c, but only slightly increase a. The results from this study suggest that the observed oscillatory zoning of jarosite-group minerals at Xitieshan resulted mainly from substitutions of K for Na at the A site and P for S at the X site.

  5. X-ray generator

    DOEpatents

    Dawson, John M.

    1976-01-01

    Apparatus and method for producing coherent secondary x-rays that are controlled as to direction by illuminating a mixture of high z and low z gases with an intense burst of primary x-rays. The primary x-rays are produced with a laser activated plasma, and these x-rays strip off the electrons of the high z atoms in the lasing medium, while the low z atoms retain their electrons. The neutral atoms transfer electrons to highly excited states of the highly striped high z ions giving an inverted population which produces the desired coherent x-rays. In one embodiment, a laser, light beam provides a laser spark that produces the intense burst of coherent x-rays that illuminates the mixture of high z and low z gases, whereby the high z atoms are stripped while the low z ones are not, giving the desired mixture of highly ionized and neutral atoms. To this end, the laser spark is produced by injecting a laser light beam, or a plurality of beams, into a first gas in a cylindrical container having an adjacent second gas layer co-axial therewith, the laser producing a plasma and the intense primary x-rays in the first gas, and the second gas containing the high and low atomic number elements for receiving the primary x-rays, whereupon the secondary x-rays are produced therein by stripping desired ions in a neutral gas and transfer of electrons to highly excited states of the stripped ions from the unionized atoms. Means for magnetically confining and stabilizing the plasma are disclosed for controlling the direction of the x-rays.

  6. Studies on solar hard X-Rays and gamma-rays: Compton backscatter, anisotropy, polarization and evidence for two phases of acceleration. Ph.D. Thesis - Maryland Univ.

    NASA Technical Reports Server (NTRS)

    Bai, T.

    1977-01-01

    Observations of solar X-rays and gamma-rays from large flares show that the hard X-ray spectrum extends into the gamma ray region, where a flattening in the spectrum of the continuum emission is observed above about 1 MeV. This emission is believed to be due to bremsstrahlung. In addition to electron-proton collisions, at energies greater than approximately 500 keV, bremsstrahlung due to electron-electron collisions becomes significant. Bremsstrahlung production was calculated for a variety of electron spectra extending from the nonrelativistic region to relativistic energies and electron-electron bremsstrahlung is taken into account. By comparing these calculations with data, it is shown that the flattening in the spectrum of the continuum emission can be best explained by an electron spectrum consisting of two distinctive components. This evidence, together with information on the X-ray and gamma ray time profiles, implied the existence of two phases of acceleration. The first phase accelerates electrons mainly up to about several hundred keV; the second phase accelerates a small fraction of the electrons accelerated in the first phase to relativistic energies and accelerates protons to tens and hundreds of MeV.

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

    Adams, Merrin S.; Dillon, Carolyn T.; Vogt, Stefan

    Metal toxicity to aquatic organisms depends on the speciation of the metal and its binding to the critical receptor site(s) (biotic ligand) of the organism. The intracellular nature of the biotic ligand for Cu in microalgal cells was investigated using the high elemental sensitivity of microprobe synchrotron radiation X-ray fluorescence (SR-XRF) and X-ray absorption near-edge spectroscopy (XANES). The marine microalgae, Ceratoneis closterium, Phaeodactylum tricornutum, and Tetraselmis sp. were selected based on their varying sensitivities to Cu (72-h 50% population growth inhibitions of 8–47 μg Cu/L). Intracellular Cu in control cells was similar for all three species (2.5–3.2 × 10–15 gmore » Cu/cell) and increased 4-fold in C. closterium and Tetraselmis sp. when exposed to copper, but was unchanged in P. tricornutum (72-h exposure to 19, 40, and 40 μg Cu/L, respectively). Whole cell microprobe SR-XRF identified endogenous Cu in the central compartment (cytoplasm) of control (unexposed) cells. After Cu exposure, Cu was colocated with organelles/granules dense in P, S, Ca, and Si and this was clearly evident in thin sections of Tetraselmis sp. XANES indicated coexistence of Cu(I) and Cu(II) in control and Cu-exposed cells, with the Cu ligand (e.g., phytochelatin) in P. tricornutum different from that in C. closterium and Tetraselmis sp. Here, this study supports the hypothesis that Cu(II) is reduced to Cu(I) and that polyphosphate bodies and phytochelatins play a significant role in the internalization and detoxification of Cu in marine microalgae.« less

  8. 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

  9. 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

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

    Fukao, Shinji; Nakanishi, Yoshikazu; Mizoguchi, Tadahiro

    X-rays are radiated due to the bremsstrahlung caused by the collision of electrons with a metal target placed opposite the negative electric surface of a crystal by changing the temperature of a LiNbO{sub 3} single crystal uniaxially polarized in the c-axis direction. It is suggested that both electric field intensity and electron density determine the intensity of X-ray radiation. Electrons are supplied by the ionization of residual gas in space, field emission from a case inside which a crystal is located, considered to be due to the high electric-field intensity formed by the surface charges on the crystal, and anmore » external electron source, such as a thermionic source. In a high vacuum, it was found that the electrons supplied by electric-field emission mainly contribute to the radiation of X-rays. It was found that the integrated intensity of X-rays can be maximized by supplying electrons both external and by electric-field emission. Furthermore, the integrated intensity of the X-rays is stable for many repeated temperature changes.« less

  11. Symposium N: Materials and Devices for Thermal-to-Electric Energy Conversion

    DTIC Science & Technology

    2010-08-24

    X - ray diffraction, transmission electron microscopy, scanning electron microscopy, and dynamic light scattering. Thermal conductivity measurements...SEM), X - ray diffraction (XRD) measurements as well as Raman spectroscopy. The results from these techniques indicate a clear modification...was examined by using scanning electron microscope (SEM; HITACHI S-4500 model) attached with an energy dispersive x - ray spectroscopy. The electrical

  12. Trajectories of high energy electrons in a plasma focus

    NASA Technical Reports Server (NTRS)

    Harries, W. L.; Lee, J. H.; Mcfarland, D. R.

    1978-01-01

    Measurements are made of high-energy electron trajectories in a plasma focus as functions of position, time, energy, and angle of emission. The spatial resolution of the X-ray emission shows that low-energy X-rays are emitted from the anode surface. It is also suggested that the highest energy X-rays originate from a small region on the axis. The so-called shadow technique shows that the electron beam is perpendicular to the anode surface. Polar diagrams of medium and high-energy X-rays agree with the bremsstrahlung emission from a relativistic electron beam, the current of which is several 100 A.

  13. Thomson-backscattered x rays from laser-accelerated electrons.

    PubMed

    Schwoerer, H; Liesfeld, B; Schlenvoigt, H-P; Amthor, K-U; Sauerbrey, R

    2006-01-13

    We present the first observation of Thomson-backscattered light from laser-accelerated electrons. In a compact, all-optical setup, the "photon collider," a high-intensity laser pulse is focused into a pulsed He gas jet and accelerates electrons to relativistic energies. A counterpropagating laser probe pulse is scattered from these high-energy electrons, and the backscattered x-ray photons are spectrally analyzed. This experiment demonstrates a novel source of directed ultrashort x-ray pulses and additionally allows for time-resolved spectroscopy of the laser acceleration of electrons.

  14. Electron beams in solar flares

    NASA Technical Reports Server (NTRS)

    Aschwanden, Markus J.; Dennis, Brian R.; Benz, Arnold O.

    1994-01-01

    A list of publications resulting from this program includes 'The Timing of Electron Beam Signatures in Hard X-Ray and Radio: Solar Flare Observations by BATSE/Compton Gamma-Ray Observatory and PHOENIX'; 'Coherent-Phase or Random-Phase Acceleration of Electron Beams in Solar Flares'; 'Particle Acceleration in Flares'; 'Chromospheric Evaporation and Decimetric Radio Emission in Solar Flares'; 'Sequences of Correlated Hard X-Ray and Type 3 Bursts During Solar Flares'; and 'Solar Electron Beams Detected in Hard X-Rays and Radiowaves.' Abstracts and reprints of each are attached to this report.

  15. Generation of High Brightness X-rays with the PLEIADES Thomson X-ray Source

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

    Brown, W J; Anderson, S G; Barty, C P J

    2003-05-28

    The use of short laser pulses to generate high peak intensity, ultra-short x-ray pulses enables exciting new experimental capabilities, such as femtosecond pump-probe experiments used to temporally resolve material structural dynamics on atomic time scales. PLEIADES (Picosecond Laser Electron InterAction for Dynamic Evaluation of Structures) is a next generation Thomson scattering x-ray source being developed at Lawrence Livermore National Laboratory (LLNL). Ultra-fast picosecond x-rays (10-200 keV) are generated by colliding an energetic electron beam (20-100 MeV) with a high intensity, sub-ps, 800 nm laser pulse. The peak brightness of the source is expected to exceed 10{sup 20} photons/s/0.1% bandwidth/mm2/mrad2. Simulationsmore » of the electron beam production, transport, and final focus are presented. Electron beam measurements, including emittance and final focus spot size are also presented and compared to simulation results. Measurements of x-ray production are also reported and compared to theoretical calculations.« less

  16. Laboratory Measurements of X-Ray Emissions From Centimeter-Long Streamer Corona Discharges

    NASA Astrophysics Data System (ADS)

    da Silva, C. L.; Millan, R. M.; McGaw, D. G.; Yu, C. T.; Putter, A. S.; LaBelle, J.; Dwyer, J.

    2017-11-01

    We provide extensive evidence that runaway electron acceleration and subsequent bremsstrahlung X-ray emission are a common feature in negative electrical discharges with voltages as low as 100 kV, indicating that all negative lightning could potentially produce runaway electrons. Centimeter long streamer corona discharges produce bursts of X-ray radiation, emitted by a source highly compact in space and time, leading to photon pileup. Median photon burst energies vary between 33 and 96 keV in 100 kV discharges. Statistical analysis of 5,000+ discharges shows that X-rays are observed in as many as 60% of the triggers, depending on the configuration. X-ray detection is more frequent when streamers are not followed by a spark, the detector is oriented perpendicular to the gap, and a thicker anode is used. In an 8-cm-long gap, X-rays are produced when runaway electrons hit the anode, and the electron acceleration is not necessarily correlated with streamer collisions.

  17. Fresh-slice multicolour X-ray free-electron lasers

    DOE PAGES

    Lutman, Alberto A.; Maxwell, Timothy J.; MacArthur, James P.; ...

    2016-10-24

    X-ray free-electron lasers (XFELs) provide femtosecond X-ray pulses with a narrow energy bandwidth and unprecedented brightness. Ultrafast physical and chemical dynamics, initiated with a site-specific X-ray pulse, can be explored using XFELs with a second ultrashort X-ray probe pulse. However, existing double-pulse schemes are complicated, difficult to customize or provide only low-intensity pulses. Here we present the novel fresh-slice technique for multicolour pulse production, wherein different temporal slices of an electron bunch lase to saturation in separate undulator sections. This method combines electron bunch tailoring from a passive wakefield device with trajectory control to provide multicolour pulses. The fresh-slice schememore » outperforms existing techniques at soft X-ray wavelengths. It produces femtosecond pulses with a power of tens of gigawatts and flexible colour separation. The pulse delay can be varied from temporal overlap to almost one picosecond. As a result, we also demonstrate the first three-colour XFEL and variably polarized two-colour pulses.« less

  18. High resolution energy-angle correlation measurement of hard x rays from laser-Thomson backscattering.

    PubMed

    Jochmann, A; Irman, A; Bussmann, M; Couperus, J P; Cowan, T E; Debus, A D; Kuntzsch, M; Ledingham, K W D; Lehnert, U; Sauerbrey, R; Schlenvoigt, H P; Seipt, D; Stöhlker, Th; Thorn, D B; Trotsenko, S; Wagner, A; Schramm, U

    2013-09-13

    Thomson backscattering of intense laser pulses from relativistic electrons not only allows for the generation of bright x-ray pulses but also for the investigation of the complex particle dynamics at the interaction point. For this purpose a complete spectral characterization of a Thomson source powered by a compact linear electron accelerator is performed with unprecedented angular and energy resolution. A rigorous statistical analysis comparing experimental data to 3D simulations enables, e.g., the extraction of the angular distribution of electrons with 1.5% accuracy and, in total, provides predictive capability for the future high brightness hard x-ray source PHOENIX (photon electron collider for narrow bandwidth intense x rays) and potential gamma-ray sources.

  19. X-ray emissions from centimeter-long streamer corona discharges

    NASA Astrophysics Data System (ADS)

    da Silva, C. L.; Millan, R. M.; McGaw, D. G.; Yu, C. T.; Putter, A. S.; Labelle, J. W.; Dwyer, J. R.

    2017-12-01

    In this work we provide extensive evidence that runaway electron acceleration and subsequent bremsstrahlung X-ray emission are a common feature in electrical discharges of negative polarity. They can be easily detected at voltages as low as 100 kV, indicating that all negative lightning could potentially produce runaway electrons. We show that centimeter-long streamer corona discharges produce bursts of X-ray radiation that are emitted by a source that is highly compact in space and time. Therefore, the emitted X-ray photons arrive together at the detector and pile up. Median burst energies vary between 33-96% of the total 100 keV available electrostatic energy that an electron can acquire in the gap. We present detailed statistical analysis of 5000+ discharges, showing that X-rays are observed in as many as 60% of the triggers, depending on the configuration. X-ray detection is more frequent when: the streamer corona discharge is not followed by a spark, the detector is oriented perpendicular to the gap, and a thicker anode is used. We show that for an 8-cm-long gap, X-rays are produced when runaway electrons hit the anode, and that the runaway electron acceleration is not correlated with streamer collisions, as inferred in meter-long discharges. The described experiment is a promising way for measuring the runaway electron distribution very close to the source and its dependence on the applied voltage.

  20. X-ray diffraction and spectroscopic study of wiluite: implications for the vesuvianite-group nomenclature

    NASA Astrophysics Data System (ADS)

    Panikorovskii, Taras L.; Mazur, Anton S.; Bazai, Ayya V.; Shilovskikh, Vladimir V.; Galuskin, Evgeny V.; Chukanov, Nikita V.; Rusakov, Vyacheslav S.; Zhukov, Yurii M.; Avdontseva, Evgenia Yu.; Aksenov, Sergey M.; Krivovichev, Sergey V.

    2017-09-01

    Two wiluite samples from the Wiluy River, Yakutia, Russia have been investigated by means of single-crystal and powder X-ray diffraction, electron microprobe analysis, 1H, 27Al, 11B, and 29Si magic-angle spinning nuclear magnetic resonance (MAS NMR), thermogravimetric analysis (DSC/TGA), X-ray photoelectron spectroscopy (XPS) at the Si2p, Ca2p, Al2p, Mg1s, B1s and Fe2p core levels, 57Fe Mössbauer spectroscopy, infrared (IR) spectroscopy and optical measurements. The crystal structures have been refined in the P4/ nnc space group [ a = 15.7027(3), c = 11.7008(3) Å, V = 2885.1(1) Å3 for 1 and a = 15.6950(2), c = 11.6787(4) Å, V = 2876.9(1) Å3 for 2] to R 1 = 0.022 and R 1 = 0.021, respectively. In the crystal structure of wiluite, five-coordinated Y1 site is predominantly occupied by Mg. IR spectra of wiluite substantially different from those of vesuvianite, in particular, by the presence of additional bands in the range 1080‒1415 cm-1, which correspond to symmetric B‒O stretching vibrations of the BO 3 3- and BO 4 5- groups. According to the MAS NMR data, tetrahedrally coordinated T1 site is occupied by B3+ with minor amounts of Al3+. The general formula of wiluite can be written as follows ( Z = 2): Ca19Mg(Al,Mg,Fe,Ti,Mn)12(B,Al,◻)5(Si2O7)4(SiO4)10(O,OH)9O2-3. The diversity of vesuvianite-group minerals is largely determined by the population of the Y1 sites. However, wiluite is characterized by the presence of additional T1 and T2 sites and should be considered as special among other vesuvianite-group minerals. The reasonability of subdivision of the wiluite subgroup within the vesuvianite group is discussed.

  1. A new endstation at the Swiss Light Source for ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy measurements of liquid solutions.

    PubMed

    Brown, Matthew A; Redondo, Amaia Beloqui; Jordan, Inga; Duyckaerts, Nicolas; Lee, Ming-Tao; Ammann, Markus; Nolting, Frithjof; Kleibert, Armin; Huthwelker, Thomas; Müächler, Jean-Pierre; Birrer, Mario; Honegger, Juri; Wetter, Reto; Wörner, Hans Jakob; van Bokhoven, Jeroen A

    2013-07-01

    A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutions and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.

  2. X-ray free-electron laser oscillator with nuclear-resonant cavity stabilization and quantum-optical applications

    DOE PAGES

    Adams, Bernhard W.; Kim, Kwang -Je

    2016-08-09

    Here, x-ray free-electron-laser oscillators with nuclear-resonant cavity stabilization (NRS-XFELO) hold the promise for providing x-rays with unprecedented coherence properties that will enable interesting quantum-optical and metrological applications. Among these are atom optics with x-ray-based optical elements providing high momentum transfer, or a frequency standard far surpassing the best state-of the-art atomic clocks.

  3. Preparation and Thermoelectric Properties of IR(sub x)Co(sub 1-x)Sb(sub 2) Alloys

    NASA Technical Reports Server (NTRS)

    Caillat, Thierry

    1995-01-01

    The preparation and characterization of the binary arsenopyrite compounds CoSb2 and IrSb2 and IrxCo1-xSb2 alloys is reported. Single crystals of CoSb2 were grown by the vertical gradient freeze technique from solution rich in antimony. Polycrystalline samples of IrSb2 and IrxCo1-xSb2 alloys were prepared by hot-pressing of prereacted elemental powders. Samples were investigated by X-ray diffractometry, microprobe analysis and density measurements. It was found that a range of solid solution exist in the system IrxCo1-xSb2 for 0.1

  4. Testing Mechanisms and Scales of Equilibrium Using Textural and Compositional Analysis of Porphyroblasts in Rocks with Heterogeneous Garnet Distributions

    NASA Astrophysics Data System (ADS)

    Ruthven, R. C.; Ketcham, R. A.; Kelly, E. D.

    2015-12-01

    Three-dimensional textural analysis of garnet porphyroblasts and electron microprobe analyses can, in concert, be used to pose novel tests that challenge and ultimately increase our understanding of metamorphic crystallization mechanisms. Statistical analysis of high-resolution X-ray computed tomography (CT) data of garnet porphyroblasts tells us the degree of ordering or randomness of garnets, which can be used to distinguish the rate-limiting factors behind their nucleation and growth. Electron microprobe data for cores, rims, and core-to-rim traverses are used as proxies to ascertain porphyroblast nucleation and growth rates, and the evolution of sample composition during crystallization. MnO concentrations in garnet cores serve as a proxy for the relative timing of nucleation, and rim concentrations test the hypothesis that MnO is in equilibrium sample-wide during the final stages of crystallization, and that concentrations have not been greatly altered by intracrystalline diffusion. Crystal size distributions combined with compositional data can be used to quantify the evolution of nucleation rates and sample composition during crystallization. This study focuses on quartzite schists from the Picuris Mountains with heterogeneous garnet distributions consisting of dense and sparse layers. 3D data shows that the sparse layers have smaller, less euhedral garnets, and petrographic observations show that sparse layers have more quartz and less mica than dense layers. Previous studies on rocks with homogeneously distributed garnet have shown that crystallization rates are diffusion-controlled, meaning that they are limited by diffusion of nutrients to growth and nucleation sites. This research extends this analysis to heterogeneous rocks to determine nucleation and growth rates, and test the assumption of rock-wide equilibrium for some major elements, among a set of compositionally distinct domains evolving in mm- to cm-scale proximity under identical P-T conditions.

  5. Biologic Rhythms Derived from Siberian Mammoths' Hairs

    PubMed Central

    Spilde, Mike; Lanzirotti, Antonio; Qualls, Clifford; Phillips, Genevieve; Ali, Abdul-Mehdi; Agenbroad, Larry; Appenzeller, Otto

    2011-01-01

    Hair is preserved for millennia in permafrost; it enshrines a record of biologic rhythms and offers a glimpse at chronobiology as it was in extinct animals. Here we compare biologic rhythms gleaned from mammoth's hairs with those of modern human hair. Four mammoths' hairs came from varying locations in Siberia 4600 km, four time zones, apart ranging in age between 18,000 and 20,000 years before present. We used two contemporaneous human hairs for comparison. Power spectra derived from hydrogen isotope ratios along the length of the hairs gave insight into biologic rhythms, which were different in the mammoths depending on location and differed from humans. Hair growth for mammoths was ∼31 cms/year and ∼16 cms/year for humans. Recurrent annual rhythms of slow and fast growth varying from 3.4 weeks/cycles to 8.7 weeks/cycles for slow periods and 1.2 weeks/cycles to 2.2 weeks/cycles for fast periods were identified in mammoth's hairs. The mineral content of mammoth's hairs was measured by electron microprobe analysis (k-ratios), which showed no differences in sulfur amongst the mammoth hairs but significantly more iron then in human hair. The fractal nature of the data derived from the hairs became evident in Mandelbrot sets derived from hydrogen isotope ratios, mineral content and geographic location. Confocal microscopy and scanning electron microscopy showed varied degrees of preservation of the cuticle largely independent of age but not location of the specimens. X-ray fluorescence microprobe and fluorescence computed micro-tomography analyses allowed evaluation of metal distribution and visualization of hollow tubes in the mammoth's hairs. Seasonal variations in iron and copper content combined with spectral analyses gave insights into variation in food intake of the animals. Biologic rhythms gleaned from power spectral plots obtained by modern methods revealed life style and behavior of extinct mega-fauna. PMID:21747920

  6. Biologic Rhythms Derived from Siberian Mammoths Hairs

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

    M Spilde; A Lanzirotti; C Qualls

    2011-12-31

    Hair is preserved for millennia in permafrost; it enshrines a record of biologic rhythms and offers a glimpse at chronobiology as it was in extinct animals. Here we compare biologic rhythms gleaned from mammoth's hairs with those of modern human hair. Four mammoths' hairs came from varying locations in Siberia 4600 km, four time zones, apart ranging in age between 18,000 and 20,000 years before present. We used two contemporaneous human hairs for comparison. Power spectra derived from hydrogen isotope ratios along the length of the hairs gave insight into biologic rhythms, which were different in the mammoths depending onmore » location and differed from humans. Hair growth for mammoths was {approx}31 cms/year and {approx}16 cms/year for humans. Recurrent annual rhythms of slow and fast growth varying from 3.4 weeks/cycles to 8.7 weeks/cycles for slow periods and 1.2 weeks/cycles to 2.2 weeks/cycles for fast periods were identified in mammoth's hairs. The mineral content of mammoth's hairs was measured by electron microprobe analysis (k-ratios), which showed no differences in sulfur amongst the mammoth hairs but significantly more iron then in human hair. The fractal nature of the data derived from the hairs became evident in Mandelbrot sets derived from hydrogen isotope ratios, mineral content and geographic location. Confocal microscopy and scanning electron microscopy showed varied degrees of preservation of the cuticle largely independent of age but not location of the specimens. X-ray fluorescence microprobe and fluorescence computed micro-tomography analyses allowed evaluation of metal distribution and visualization of hollow tubes in the mammoth's hairs. Seasonal variations in iron and copper content combined with spectral analyses gave insights into variation in food intake of the animals. Biologic rhythms gleaned from power spectral plots obtained by modern methods revealed life style and behavior of extinct mega-fauna.« less

  7. Biologic rhythms derived from Siberian mammoths' hairs.

    PubMed

    Spilde, Mike; Lanzirotti, Antonio; Qualls, Clifford; Phillips, Genevieve; Ali, Abdul-Mehdi; Agenbroad, Larry; Appenzeller, Otto

    2011-01-01

    Hair is preserved for millennia in permafrost; it enshrines a record of biologic rhythms and offers a glimpse at chronobiology as it was in extinct animals. Here we compare biologic rhythms gleaned from mammoth's hairs with those of modern human hair. Four mammoths' hairs came from varying locations in Siberia 4600 km, four time zones, apart ranging in age between 18,000 and 20,000 years before present. We used two contemporaneous human hairs for comparison. Power spectra derived from hydrogen isotope ratios along the length of the hairs gave insight into biologic rhythms, which were different in the mammoths depending on location and differed from humans. Hair growth for mammoths was ∼31 cms/year and ∼16 cms/year for humans. Recurrent annual rhythms of slow and fast growth varying from 3.4 weeks/cycles to 8.7 weeks/cycles for slow periods and 1.2 weeks/cycles to 2.2 weeks/cycles for fast periods were identified in mammoth's hairs. The mineral content of mammoth's hairs was measured by electron microprobe analysis (k-ratios), which showed no differences in sulfur amongst the mammoth hairs but significantly more iron then in human hair. The fractal nature of the data derived from the hairs became evident in Mandelbrot sets derived from hydrogen isotope ratios, mineral content and geographic location. Confocal microscopy and scanning electron microscopy showed varied degrees of preservation of the cuticle largely independent of age but not location of the specimens. X-ray fluorescence microprobe and fluorescence computed micro-tomography analyses allowed evaluation of metal distribution and visualization of hollow tubes in the mammoth's hairs. Seasonal variations in iron and copper content combined with spectral analyses gave insights into variation in food intake of the animals. Biologic rhythms gleaned from power spectral plots obtained by modern methods revealed life style and behavior of extinct mega-fauna.

  8. Modification and benchmarking of MCNP for low-energy tungsten spectra.

    PubMed

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

    2000-12-01

    The MCNP Monte Carlo radiation transport code was modified for diagnostic medical physics applications. In particular, the modified code was thoroughly benchmarked for the production of polychromatic tungsten x-ray spectra in the 30-150 kV range. Validating the modified code for coupled electron-photon transport with benchmark spectra was supplemented with independent electron-only and photon-only transport benchmarks. Major revisions to the code included the proper treatment of characteristic K x-ray production and scoring, new impact ionization cross sections, and new bremsstrahlung cross sections. Minor revisions included updated photon cross sections, electron-electron bremsstrahlung production, and K x-ray yield. The modified MCNP code is benchmarked to electron backscatter factors, x-ray spectra production, and primary and scatter photon transport.

  9. Density gradient free electron collisionally excited x-ray laser

    DOEpatents

    Campbell, E.M.; Rosen, M.D.

    1984-11-29

    An operational x-ray laser is provided that amplifies 3p-3s transition x-ray radiation along an approximately linear path. The x-ray laser is driven by a high power optical laser. The driving line focused optical laser beam illuminates a free-standing thin foil that may be associated with a substrate for improved structural integrity. This illumination produces a generally cylindrically shaped plasma having an essentially uniform electron density and temperature, that exists over a long period of time, and provides the x-ray laser gain medium. The x-ray laser may be driven by more than one optical laser beam. The x-ray laser has been successfully demonstrated to function in a series of experimental tests.

  10. Status of the eROSITA Telescope testing and calibrating the x-ray mirror assemblies

    NASA Astrophysics Data System (ADS)

    Burwitz, Vadim; Predehl, Peter; Bräuninger, Heinrich; Burkert, Wolfgang; Dennerl, Konrad; Eder, Josef; Friedrich, Peter; Fürmetz, Maria; Grisoni, Gabriele; Hartner, Gisela; Marioni, Fabio; Menz, Benedikt; Pfeffermann, Elmar; Valsecchi, Giuseppe

    2013-09-01

    The eROSITA X-ray observatory that will be launched on board the Russian Spectrum-RG mission comprises seven X-ray telescopes, each with its own mirror assembly (mirror module + X-ray baffle), electron deflector, filter wheel, and CCD camera with its control electronics. The completed flight mirror modules are undergoing many thorough X-ray tests at the PANTHER X-ray test facility after delivery, after being mated with the X-ray baffle, and again after both the vibration and thermal-vacuum tests. A description of the work done with mirror modules/assemblies and the test results obtained will be reported here. We report also on the environmental tests that have been performed on the eROSITA telescope qualification model.

  11. LABORATORY MEASUREMENTS COMPELLINGLY SUPPORT A CHARGE-EXCHANGE MECHANISM FOR THE “DARK MATTER” ∼3.5 keV X-Ray LINE

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

    Shah, Chintan; Dobrodey, Stepan; Bernitt, Sven

    2016-12-10

    The reported observations of an unidentified X-ray line feature at ∼3.5 keV have driven a lively discussion about its possible dark matter origin. Motivated by this, we have measured the K-shell X-ray spectra of highly ionized bare sulfur ions following charge exchange with gaseous molecules in an electron beam ion trap, as a source of or a contributor to this X-ray line. We produced S{sup 16+} and S{sup 15+} ions and let them capture electrons in collision with those molecules with the electron beam turned off while recording X-ray spectra. We observed a charge-exchange-induced X-ray feature at the Lyman seriesmore » limit (3.47 ± 0.06 keV). The inferred X-ray energy is in full agreement with the reported astrophysical observations and supports the novel scenario proposed by Gu et al.« less

  12. Radiation damage free ghost diffraction with atomic resolution

    DOE PAGES

    Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

    2017-12-21

    The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

  13. Radiation damage free ghost diffraction with atomic resolution

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

    Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

    The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

  14. Development of a low-energy x-ray camera for the imaging of secondary electron bremsstrahlung x-ray emitted during proton irradiation for range estimation.

    PubMed

    Ando, Koki; Yamaguchi, Mitsutaka; Yamamoto, Seiichi; Toshito, Toshiyuki; Kawachi, Naoki

    2017-06-21

    Imaging of secondary electron bremsstrahlung x-ray emitted during proton irradiation is a possible method for measurement of the proton beam distribution in phantom. However, it is not clear that the method is used for range estimation of protons. For this purpose, we developed a low-energy x-ray camera and conducted imaging of the bremsstrahlung x-ray produced during irradiation of proton beams. We used a 20 mm  ×  20 mm  ×  1 mm finely grooved GAGG scintillator that was optically coupled to a one-inch square high quantum efficiency (HQE)-type position-sensitive photomultiplier tube to form an imaging detector. The imaging detector was encased in a 2 cm-thick tungsten container, and a pinhole collimator was attached to its camera head. After performance of the camera was evaluated, secondary electron bremsstrahlung x-ray imaging was conducted during irradiation of the proton beams for three different proton energies, and the results were compared with Monte Carlo simulation as well as calculated value. The system spatial resolution and sensitivity of the developed x-ray camera with 1.5 mm-diameter pinhole collimator were estimated to be 32 mm FWHM and 5.2  ×  10 -7 for ~35 keV x-ray photons at 100 cm from the collimator surface, respectively. We could image the proton beam tracks by measuring the secondary electron bremsstrahlung x-ray during irradiation of the proton beams, and the ranges for different proton energies could be estimated from the images. The measured ranges from the images were well matched with the Monte Carlo simulation, and slightly smaller than the calculated values. We confirmed that the imaging of the secondary electron bremsstrahlung x-ray emitted during proton irradiation with the developed x-ray camera has the potential to be a new tool for proton range estimations.

  15. Electronic structure and soft-X-ray-induced photoreduction studies of iron-based magnetic polyoxometalates of type {(M)M5}12Fe(III)30 (M = Mo(VI), W(VI)).

    PubMed

    Kuepper, Karsten; Derks, Christine; Taubitz, Christian; Prinz, Manuel; Joly, Loïc; Kappler, Jean-Paul; Postnikov, Andrei; Yang, Wanli; Kuznetsova, Tatyana V; Wiedwald, Ulf; Ziemann, Paul; Neumann, Manfred

    2013-06-14

    Giant Keplerate-type molecules with a {Mo72Fe30} core show a number of very interesting properties, making them particularly promising for various applications. So far, only limited data on the electronic structure of these molecules from X-ray spectra and electronic structure calculations have been available. Here we present a combined electronic and magnetic structure study of three Keplerate-type nanospheres--two with a {Mo72Fe30} core and one with a {W72Fe30} core by means of X-ray absorption spectroscopy, X-ray magnetic circular dichroism (XMCD), SQUID magnetometry, and complementary theoretical approaches. Furthermore, we present detailed studies of the Fe(3+)-to-Fe(2+) photoreduction process, which is induced under soft X-ray radiation in these molecules. We observe that the photoreduction rate greatly depends on the ligand structure surrounding the Fe ions, with negatively charged ligands leading to a dramatically reduced photoreduction rate. This opens the possibility of tailoring such polyoxometalates by X-ray spectroscopic studies and also for potential applications in the field of X-ray induced photochemistry.

  16. Nonlinear effects in propagation of radiation of X-ray free-electron lasers

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

    Nosik, V. L., E-mail: v-nosik@yandex.ru, E-mail: nosik@ns.crys.ras.ru

    2016-05-15

    Nonlinear effects accompanying the propagation of high-intensity beams of X-ray free-electron lasers are considered. It is shown that the X-ray wave field in the crystal significantly changes due to the formation of “hollow” atomic shells as a result of the photoelectric effect.

  17. An investigation on some of the tumor treatment cases using x-rays and electron beams

    NASA Astrophysics Data System (ADS)

    Ucar, Burcu; Yigitoglu, Ibrahim; Arslan Kabalay, Ipek; Altiparmak, Duygu; Kilicaslan, Sinem

    2015-07-01

    In this work, we discussed some of the applications which X-rays and electron beam used in radiotherapy for tumor treatments. This study has been performed at Radiation Oncology Department, Medicine Faculty in Gaziosmanpasa University by using the VARIAN CLINICA DHX linear accelerator which is operated in the range of 6 MeV - 15 MeV. Processes for the treatments that X-rays used for pancreas, bladder and prostate tumors and the processes that the electron beam used for some of the derm tumors are studied. Effects of X-rays and electron beams to treatments process are examined and the obtained results are presented comparatively.

  18. Energetics of impulsive solar flares: Correlating BATSE hard x-ray bursts and the solar atmosphere's soft x-ray response

    NASA Technical Reports Server (NTRS)

    Newton, Elizabeth

    1996-01-01

    This investigation has involved the correlation of BATSE-observed solar hard X-ray emission with the characteristics of soft X-ray emitting plasma observed by the Yohkoh Bragg Crystal Spectrometers. The goal was to test the hypothesis that localized electron beam heating is the dominant energy transport mechanism in impulsive flares, as formulated in the thick-target electron-heated model of Brown.

  19. Two-dimensional time-resolved ultra-high speed imaging of K-alpha emission from short-pulse-laser interactions to observe electron recirculation

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

    Nagel, S. R.; Chen, H.; Park, J.

    Time resolved x-ray images with 7 ps resolution are recorded on relativistic short-pulse laser-plasma experiments using the dilation x-ray imager, a high-speed x-ray framing camera, sensitive to x-rays in the range of ≈1-17 keV. Furthermore, this capability enables a series of 2D x-ray images to be recorded at picosecond scales, which allows for the investigation of fast electron transport within the target with unprecedented temporal resolution. With an increase in the Kα-emission spot size over time we found that targets were thinner than the recirculation limit and is absent for thicker targets. Together with the observed polarization dependence of themore » spot size increase, this indicates that electron recirculation is relevant for the x-ray production in thin targets.« less

  20. Two-dimensional time-resolved ultra-high speed imaging of K-alpha emission from short-pulse-laser interactions to observe electron recirculation

    DOE PAGES

    Nagel, S. R.; Chen, H.; Park, J.; ...

    2017-04-04

    Time resolved x-ray images with 7 ps resolution are recorded on relativistic short-pulse laser-plasma experiments using the dilation x-ray imager, a high-speed x-ray framing camera, sensitive to x-rays in the range of ≈1-17 keV. Furthermore, this capability enables a series of 2D x-ray images to be recorded at picosecond scales, which allows for the investigation of fast electron transport within the target with unprecedented temporal resolution. With an increase in the Kα-emission spot size over time we found that targets were thinner than the recirculation limit and is absent for thicker targets. Together with the observed polarization dependence of themore » spot size increase, this indicates that electron recirculation is relevant for the x-ray production in thin targets.« less

  1. 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.

  2. X-Ray Data Booklet

    Science.gov Websites

    X-RAY DATA BOOKLET Center for X-ray Optics and Advanced Light Source Lawrence Berkeley National Laboratory Introduction X-Ray Properties of Elements Electron Binding Energies X-Ray Energy Emission Energies Table of X-Ray Properties Synchrotron Radiation Characteristics of Synchrotron Radiation History of X

  3. High Energy Electron Detectors on Sphinx

    NASA Astrophysics Data System (ADS)

    Thompson, J. R.; Porte, A.; Zucchini, F.; Calamy, H.; Auriel, G.; Coleman, P. L.; Bayol, F.; Lalle, B.; Krishnan, M.; Wilson, K.

    2008-11-01

    Z-pinch plasma radiation sources are used to dose test objects with K-shell (˜1-4keV) x-rays. The implosion physics can produce high energy electrons (> 50keV), which could distort interpretation of the soft x-ray effects. We describe the design and implementation of a diagnostic suite to characterize the electron environment of Al wire and Ar gas puff z-pinches on Sphinx. The design used ITS calculations to model detector response to both soft x-rays and electrons and help set upper bounds to the spurious electron flux. Strategies to discriminate between the known soft x-ray emission and the suspected electron flux will be discussed. H.Calamy et al, ``Use of microsecond current prepulse for dramatic improvements of wire array Z-pinch implosion,'' Phys Plasmas 15, 012701 (2008) J.A.Halbleib et al, ``ITS: the integrated TIGER series of electron/photon transport codes-Version 3.0,'' IEEE Trans on Nuclear Sci, 39, 1025 (1992)

  4. Prediction and observation of tin and silver plasmas with index of refraction greater than one in the soft x-ray range.

    PubMed

    Filevich, Jorge; Grava, Jonathan; Purvis, Mike; Marconi, Mario C; Rocca, Jorge J; Nilsen, Joseph; Dunn, James; Johnson, Walter R

    2006-07-01

    We present the calculated prediction and the experimental confirmation that doubly ionized Ag and Sn plasmas can have an index of refraction greater than one for soft x-ray wavelengths. Interferometry experiments conducted using a capillary discharge soft x-ray laser operating at a wavelength of confirm that in few times ionized laser-created plasmas of these elements the anomalous dispersion from bound electrons can dominate the free electron contribution, making the index of refraction greater than one. The results confirm that bound electrons can strongly influence the index of refraction of numerous plasmas over a broad range of soft x-ray wavelengths confirming recent observations. The understanding of index of refraction at short wavelengths will become even more essential during the next decade as x-ray free electron lasers will become available to probe a wider variety of plasmas at higher densities and shorter wavelengths.

  5. Implications of X-Ray Observations for Electron Acceleration and Propagation in Solar Flares

    NASA Technical Reports Server (NTRS)

    Holman, G. D.; Aschwanden, M. J.; Aurass, H.; Battaglia, M.; Grigis, P. C.; Kontar, E. P.; Liu, W.; Saint-Hilaire, P.; Zharkova, V. V.

    2011-01-01

    High-energy X-rays and gamma-rays from solar flares were discovered just over fifty years ago. Since that time, the standard for the interpretation of spatially integrated flare X-ray spectra at energies above several tens of keV has been the collisional thick-target model. After the launch of the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI) in early 2002, X-ray spectra and images have been of sufficient quality to allow a greater focus on the energetic electrons responsible for the X-ray emission, including their origin and their interactions with the flare plasma and magnetic field. The result has been new insights into the flaring process, as well as more quantitative models for both electron acceleration and propagation, and for the flare environment with which the electrons interact. In this article we review our current understanding of electron acceleration, energy loss, and propagation in flares. Implications of these new results for the collisional thick-target model, for general flare models, and for future flare studies are discussed.

  6. 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.

  7. Monoclinic tridymite in clast-rich impact melt rock from the Chesapeake Bay impact structure

    USGS Publications Warehouse

    Jackson, John C.; Horton, J. Wright; Chou, I-Ming; Belkin, Harvey E.

    2011-01-01

    X-ray diffraction and Raman spectroscopy confirm a rare terrestrial occurrence of monoclinic tridymite in clast-rich impact melt rock from the Eyreville B drill core in the Chesapeake Bay impact structure. The monoclinic tridymite occurs with quartz paramorphs after tridymite and K-feldspar in a microcrystalline groundmass of devitrified glass and Fe-rich smectite. Electron-microprobe analyses revealed that the tridymite and quartz paramorphs after tridymite contain different amounts of chemical impurities. Inspection by SEM showed that the tridymite crystal surfaces are smooth, whereas the quartz paramorphs contain irregular tabular voids. These voids may represent microporosity formed by volume decrease in the presence of fluid during transformation from tridymite to quartz, or skeletal growth in the original tridymite. Cristobalite locally rims spherulites within the same drill core interval. The occurrences of tridymite and cristobalite appear to be restricted to the thickest clast-rich impact melt body in the core at 1402.02–1407.49 m depth. Their formation and preservation in an alkali-rich, high-silica melt rock suggest initially high temperatures followed by rapid cooling.

  8. Crystal Chemistry of Pyroaurite from the Kovdor Pluton, Kola Peninsula, Russia, and the Långban Fe-Mn deposit, Värmland, Sweden

    NASA Astrophysics Data System (ADS)

    Zhitova, E. S.; Ivanyuk, G. Yu.; Krivovichev, S. V.; Yakovenchuk, V. N.; Pakhomovsky, Ya. A.; Mikhailova, Yu. A.

    2017-12-01

    Pyroaurite [Mg6Fe2 3+ (OH)16][(CO3)(H2O)] from the Kovdor Pluton on the Kola Peninsula, Russia, and the Långban deposit in Filipstad, Värmland, Sweden were studied with single crystal and powder X-ray diffraction, an electron microprobe, and Raman spectroscopy. Both samples are rhombohedral, space group R3̅ m, a = 3.126(3), c = 23.52(2) Å (Kovdor), and a = 3.1007(9), c = 23.34(1) (Långban). The powder XRD revealed only the 3 R polytype. The ratio of di- and trivalent cations M 2+: M 3+ was determined as 3.1-3.2 (Kovdor) and 3.0 (Långban). The Raman spectroscopy of the Kovdor sample verified hydroxyl groups and/or water molecules in the mineral (absorption bands in the region of 3600-3500 cm-1) and carbonate groups (absorption bands in the region of 1346-1058 cm-1). Based on the data obtained, the studied samples should be identified as pyroaurite-3 R (hydrotalcite group).

  9. Oxidation and corrosion resistance of candidate Stirling engine heater-head-tube alloys

    NASA Technical Reports Server (NTRS)

    Stephens, J. R.; Barrett, C. A.

    1984-01-01

    Sixteen candidate iron base Stirling engine heater head tube alloys are evaluated in a diesel fuel fired simulator materials test rig to determine their oxidation and corrosion resistance. Sheet specimens are tested at 820 C for 3500 hr in 5 hr heating cycles. Specific weight change data and an attack parameter are used to categorize the alloys into four groups; 10 alloys show excellent for good oxidation and corrosion resistance and six alloys exhibit poor or catastrophic resistance. Metallographic, X-ray, and electron microprobe analyses aid in further characterizing the oxidation and corrosion behavior of the alloys. Alloy compositions, expecially the reactive elements aluminum, titanium, and chromium, play a major role in the excellent oxidation and corrosion behavior of the alloys. The best oxidation resistance is associated with the formation of an iron nickel aluminum outer oxide scale, an intermediate oxide scale rich in chromium and titanium, and an aluminum outer oxide scale adjacent to the metallic substrate, which exhibits a zone of internal oxidation of aluminum and to some extent titanium.

  10. The first investigative science-based evidence of Morgellons psychogenesis.

    PubMed

    Roncati, Luca; Gatti, Antonietta Morena; Pusiol, Teresa; Piscioli, Francesco; Barbolini, Giuseppe; Maiorana, Antonio

    2016-01-01

    Morgellons disease is an infrequent syndromic condition, that typically affects middle-aged white women, characterized by crawling sensations on and under the skin, associated with itchy rashes, stinging sores, fiber-like filaments emerging from the sores, severe fatigue, concentrating difficulty, and memory loss. The scientific community is prone to believe that Morgellons is the manifestation of various psychiatric syndromes (Munchausen, Munchausen by proxy, Ekbom, Wittmaack-Ekbom). Up until now, no investigative science-based evidence about its psychogenesis has ever been provided. In order to close this gap, we have analyzed the filaments extracted from the skin lesions of a 49-year-old Caucasian female patient, by using a Field Emission Gun-Environmental Electron Scanning Microscope equipped with an X-ray microprobe, for the chemico-elemental characterization of the filaments, comparing them with those collected during a detailed indoor investigation, with careful air monitoring, in her apartment. Our results prove the self-introduction under the epidermis of environmental filaments. For the first time in the literature, we have scientifically demonstrated the self-induced nature of Morgellons disease, thereby wiping out fanciful theories about its etiopathogenesis.

  11. The formation of hydrogen permeation barriers on steels by aluminising

    NASA Astrophysics Data System (ADS)

    Forcey, K. S.; Ross, D. K.; Wu, C. H.

    1991-06-01

    An extensive investigation has been carried out into the effectiveness of aluminised layers as permeation barriers on AISI 316L stainless and DIN 1.4914 martensitic steels. The study involved measurement of the hydrogen permeation rate through commercially aluminised steel discs of thicknesses in the range 1-1.6 mm, at temperatures between 250 and 600 °C and for an upstream hydrogen pressure of 10 5 Pa. The composition and structure of the aluminide layers were investigated by a number of techniques such as SEM, electron beam microprobe and X-ray diffraction. Accelerator based techniques such as RBS and NRA were employed to study the top micron or so of the surfaces of the samples. By these techniques it was found that the effectiveness of the permeation barrier depended on the formation of a thin surface oxide layer consisting of Al 2O 3. It was found that the permeation rate through the aluminised steels could be reduced by 3-4 orders of magnitude by forming a surface oxide layer up to a micron or so in thickness.

  12. NWA 2736: An Unusual New Graphite-bearing Aubrite

    NASA Technical Reports Server (NTRS)

    Lowe, J. J.; Hill, D. H.; Domanik, K. J.; Lauretta, D. S.; Drake, M. J.; Killgore, M.

    2005-01-01

    Aubrites are enstatite-rich achondrites that are probably related to enstatite chondrite parent bodies. The exact link, if any, is not understood. They may have formed from melting within one or more enstatite chondrite parent bodies. Description of NWA 2736: One complete stone weighing 171.51 grams was recovered from the Sahara Desert by nomads sometime before September 2004. It was completely covered with fusion crust and desert varnish. This stone is severely weathered, with caramel brown coloration throughout and calcite veins that extend into the interior of the sample. Mineral analyses were performed and elemental x-ray maps were obtained with a CAMECA SX-50 electron microprobe at the Lunar and Planetary Laboratory at the University of Arizona. The relatively high modal abundance of albitic plagioclase, presence of euhedral graphite, depletion of troilite, and occurrence of pervasive kamacite veins (some with daubreelite) all indicate that NWA 2736 has a complex history and may sample a new region of the aubrite parent body. A discussion and analysis on the overall texture of NWA 2736 is presented.

  13. Chemical reactions involved in the initiation of hot corrosion of IN-738

    NASA Technical Reports Server (NTRS)

    Fryburg, G. C.; Kohl, F. J.; Stearns, C. A.

    1984-01-01

    Sodium-sulfate-induced hot corrosion of preoxidized IN-738 was studied at 975 C with special emphasis placed on the processes occurring during the long induction period. Thermogravimetric tests were run for predetermined periods of time, and then one set of specimens was washed with water. Chemical analysis of the wash solutions yielded information about water soluble metal salts and residual sulfate. A second set of samples was cross sectioned dry and polished in a nonaqueous medium. Element distributions within the oxide scale were obtained from electron microprobe X-ray micrographs. Evolution of SO was monitored throughout the thermogravimetric tests. Kinetic rate studies were performed for several pertinent processes; appropriate rate constants were obtained from the following chemical reactions; Cr203 + 2 Na2S04(1) + 3/2 02 yields 2 Na2Cr04(1) + 2 S03(g)n TiO2 + Na2S04(1) yields Na20(T102)n + 503(g)n T102 + Na2Cro4(1) yields Na2(T102)n + Cr03(g).

  14. Characterization of the interface between the bulk glass forming alloy Zr{sub 41}Ti{sub 14}Cu{sub 12}Ni{sub 10}Be{sub 23} with pure metals and ceramics

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

    Schroers, Jan; Samwer, Konrad; Szuecs, Frigyes

    The reaction of the bulk glass forming alloy Zr{sub 41}Ti{sub 14}Cu{sub 12}Ni{sub 10}Be{sub 23} (Vit 1) with W, Ta, Mo, AlN, Al{sub 2}O{sub 3}, Si, graphite, and amorphous carbon was investigated. Vit 1 samples were melted and subsequently solidified after different processing times on discs of the different materials. Sessile drop examinations of the macroscopic wetting of Vit 1 on the discs as a function of temperature were carried out in situ with a digital optical camera. The reactions at the interfaces between the Vit 1 sample and the different disc materials were investigated with an electron microprobe. The structuremore » and thermal stability of the processed Vit 1 samples were examined by x-ray diffraction and differential scanning calorimetry. The results are discussed in terms of possible applications for composite materials. (c) 2000 Materials Research Society.« less

  15. Mode of occurrence of chromium in four US coals

    USGS Publications Warehouse

    Huggins, Frank E.; Shah, N.; Huffman, G.P.; Kolker, A.; Crowley, S.; Palmer, C.A.; Finkelman, R.B.

    2000-01-01

    The mode of occurrence of chromium in three US bituminous coals and one US subbituminous has been examined using both X-ray absorption fine structure (XAFS) spectroscopy and a selective leaching protocol supplemented by scanning electron microscopy (SEM) and electron microprobe measurements. A synthesis of results from both methods indicates that chromium occurs principally in two forms in the bituminous coals: the major occurrence of chromium is associated with the macerals and is not readily leached by any reagent, whereas a second, lesser occurrence, which is leachable in hydrofluoric acid (HF), is associated with the clay mineral, illite. The former occurrence is believed to be a small particle oxyhydroxide phase (CrO(OH)). One coal also contained a small fraction (<5%) of the chromium in the form of a chromian magnetite, and the leaching protocol indicated the possibility of a similar small fraction of chromium in sulfide form in all three coals. There was little agreement between the two techniques on the mode of occurrence of chromium in the subbituminous coal; however, only a limited number of subbituminous coals have been analyzed by either technique. The chromium in all four coals was trivalent as no evidence was found for the Cr6+ oxidation state in any coal.

  16. Microstructure Evolution During Stainless Steel-Copper Vacuum Brazing with a Ag/Cu/Pd Filler Alloy: Effect of Nickel Plating

    NASA Astrophysics Data System (ADS)

    Choudhary, R. K.; Laik, A.; Mishra, P.

    2017-03-01

    Vacuum brazing of stainless steel and copper plates was done using a silver-based filler alloy. In one set of experiments, around 30-µm-thick nickel coatings were electrochemically applied on stainless steel plates before carrying out the brazing runs and its effect in making changes in the braze-zone microstructure was studied. For brazing temperature of 830 °C, scanning electron microscopy examination of the braze-zone revealed that relatively sound joints were obtained when brazing was done with nickel-coated stainless steel than with uncoated one. However, when brazing of nickel-coated stainless steel and copper plates was done at 860 °C, a wide crack appeared in the braze-zone adjacent to copper side. Energy-dispersive x-ray analysis and electron microprobe analysis confirmed that at higher temperature, the diffusion of Cu atoms from copper plate towards the braze-zone was faster than that of Ni atoms from nickel coating. Helium leak rate of the order 10-11 Pa m3/s was obtained for the crack-free joint, whereas this value was higher than 10-4 Pa m3/s for the joint having crack. The shear strength of the joint was found to decrease considerably due to the presence of crack.

  17. Timescales of magmatic processes prior to the ˜4.7 ka Agnano-Monte Spina eruption (Campi Flegrei caldera, Southern Italy) based on diffusion chronometry from sanidine phenocrysts

    NASA Astrophysics Data System (ADS)

    Iovine, Raffaella Silvia; Fedele, Lorenzo; Mazzeo, Fabio Carmine; Arienzo, Ilenia; Cavallo, Andrea; Wörner, Gerhard; Orsi, Giovanni; Civetta, Lucia; D'Antonio, Massimo

    2017-02-01

    Barium diffusion chronometry applied to sanidine phenocrysts from the trachytic Agnano-Monte Spina eruption (˜4.7 ka) constrains the time between reactivation and eruption of magma batches in the Campi Flegrei caldera. Backscattered electron imaging and quantitative electron microprobe measurements on 50 sanidine phenocrysts from representative pumice samples document core-to-rim compositional zoning. We focus on compositional breaks near the crystal rims that record magma mixing processes just prior to eruption. Diffusion times were modeled at a magmatic temperature of 930 °C using profiles based on quantitative BaO point analyses, X-ray scans, and grayscale swath profiles, yielding times ≤60 years between mixing and eruption. Such short timescales are consistent with volcanological and geochronological data that indicate that at least six eruptions occurred in the Agnano-San Vito area during few centuries before the Agnano-Monte Spina eruption. Thus, the short diffusion timescales are similar to time intervals between eruptions. Therefore, the rejuvenation time of magma residing in a shallow reservoir after influx of a new magma batch that triggered the eruption, and thus pre-eruption warning times, may be as short as years to a few decades at Campi Flegrei caldera.

  18. Laboratory-size three-dimensional x-ray microscope with Wolter type I mirror optics and an electron-impact water window x-ray source

    NASA Astrophysics Data System (ADS)

    Ohsuka, Shinji; Ohba, Akira; Onoda, Shinobu; Nakamoto, Katsuhiro; Nakano, Tomoyasu; Miyoshi, Motosuke; Soda, Keita; Hamakubo, Takao

    2014-09-01

    We constructed a laboratory-size three-dimensional water window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques, and observed bio-medical samples to evaluate its applicability to life science research fields. It consists of a condenser and an objective grazing incidence Wolter type I mirror, an electron-impact type oxygen Kα x-ray source, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit of around 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm scale three-dimensional fine structures were resolved.

  19. Mechanical design of thin-film diamond crystal mounting apparatus for coherence preservation hard x-ray optics

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

    Shu, Deming, E-mail: shu@aps.anl.gov; Shvyd’ko, Yuri V.; Stoupin, Stanislav

    2016-07-27

    A new thin-film diamond crystal mounting apparatus has been designed at the Advanced Photon Source (APS) for coherence preservation hard x-ray optics with optimized thermal contact and minimized crystal strain. This novel mechanical design can be applied to new development in the field of: x-ray optics cavities for hard x-ray free-electron laser oscillators (XFELOs), self-seeding monochromators for hard x-ray free-electron laser (XFEL) with high average thermal loading, high heat load diamond crystal monochromators and beam-sharing/beam-split-and-delay devices for XFEL facilities and future upgraded high-brightness coherent x-ray source in the MBA lattice configuration at the APS.

  20. Laboratory-size three-dimensional x-ray microscope with Wolter type I mirror optics and an electron-impact water window x-ray source.

    PubMed

    Ohsuka, Shinji; Ohba, Akira; Onoda, Shinobu; Nakamoto, Katsuhiro; Nakano, Tomoyasu; Miyoshi, Motosuke; Soda, Keita; Hamakubo, Takao

    2014-09-01

    We constructed a laboratory-size three-dimensional water window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques, and observed bio-medical samples to evaluate its applicability to life science research fields. It consists of a condenser and an objective grazing incidence Wolter type I mirror, an electron-impact type oxygen Kα x-ray source, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit of around 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm scale three-dimensional fine structures were resolved.

  1. The Effects of Low- and High-Energy Cutoffs on Solar Flare Microwave and Hard X-Ray Spectra

    NASA Technical Reports Server (NTRS)

    Holman, G. D.; Oegerle, William (Technical Monitor)

    2002-01-01

    Microwave and hard x-ray spectra provide crucial information about energetic electrons and their environment in solar flares. These spectra are becoming better determined with the Owens Valley Solar Array (OVSA) and the recent launch of the Ramaty High Energy Solar Spectroscopic Imager (RHESSI). The proposed Frequency Agile Solar Radiotelescope (FASR) promises even greater advances in radio observations of solar flares. Both microwave and hard x-ray spectra are sensitive to cutoffs in the electron distribution function. The determination of the high-energy cutoff from these spectra establishes the highest electron energies produced by the acceleration mechanism, while determination of the low-energy cutoff is crucial to establishing the total energy in accelerated electrons. This paper will show computations of the effects of both high- and low-energy cutoffs on microwave and hard x-ray spectra. The optically thick portion of a microwave spectrum is enhanced and smoothed by a low-energy cutoff, while a hard x-ray spectrum is flattened below the cutoff energy. A high-energy cutoff steepens the microwave spectrum and increases the wavelength at which the spectrum peaks, while the hard x-ray spectrum begins to steepen at photon energies roughly an order of magnitude below the electron cutoff energy. This work discusses how flare microwave and hard x-ray spectra can be analyzed together to determine these electron cutoff energies. This work is supported in part by the NASA Sun-Earth Connection Program.

  2. 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.

  3. 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.

  4. Density gradient free electron collisionally excited X-ray laser

    DOEpatents

    Campbell, Edward M.; Rosen, Mordecai D.

    1989-01-01

    An operational X-ray laser (30) is provided that amplifies 3p-3s transition X-ray radiation along an approximately linear path. The X-ray laser (30) is driven by a high power optical laser. The driving line focused optical laser beam (32) illuminates a free-standing thin foil (34) that may be associated with a substrate (36) for improved structural integrity. This illumination produces a generally cylindrically shaped plasma having an essentially uniform electron density and temperature, that exists over a long period of time, and provides the X-ray laser gain medium. The X-ray laser (30) may be driven by more than one optical laser beam (32, 44). The X-ray laser (30) has been successfully demonstrated to function in a series of experimental tests.

  5. Combined use of infrared and hard X-ray microprobes for spectroscopy-based neuroanatomy

    NASA Astrophysics Data System (ADS)

    Surowka, A. D.; Ziomber, A.; Czyzycki, M.; Migliori, A.; Pieklo, L.; Kasper, K.; Szczerbowska-Boruchowska, M.

    2018-05-01

    Understanding the pathological triggers that affect the structural and physiological integrity of biochemical milieu of neurons is crucial to extend our knowledge on brain disorders, that are in many circumstances hardly treatable. Over recently, by using sophisticated hyperspectral micro-imaging modalities, it has been placed within our reach to get an insight into high fidelity histological details along with corresponding biochemical information in a label-free fashion, without using any additional chemical fixatives. However, in order to push forwards extensive application of these methods in the clinical arena, it is viable to make further iterations in novel data analysis protocols in order to boost their sensitivity. Therefore, in our study we proposed a new combined approach utilizing both benchtop Fourier transform infrared (FTIR) and synchrotron X-ray fluorescence (SR-XRF) micro-spectroscopies coupled with multivariate data clustering using the K-means algorithm for combined molecular and elemental micro-imaging, so that these complimentary analytical tools could be used for delineating between various brain structures based on their biochemical composition. By utilizing mid-IR transmission FTIR experiments, the biochemical composition in terms of lipids, proteins and phosphodiesters became accessible. In turn, the SR-XRF experiment was carried out at the advanced IAEA X-ray spectrometry station at Elettra Sincrotrone Trieste. By measuring in vacuum and by using the primary exciting X-ray beam, monochromatized to 10.5 keV, we took advantage of accessing the characteristic X-ray lines of a variety of elements ranging from carbon to zinc. Herein, we can report that the developed methodology has high specificity for label-free discriminating between lipid- and protein-rich brain tissue areas.

  6. Speciation of metal(loid)s in environmental samples by X-ray absorption spectroscopy: a critical review.

    PubMed

    Gräfe, Markus; Donner, Erica; Collins, Richard N; Lombi, Enzo

    2014-04-25

    Element specificity is one of the key factors underlying the widespread use and acceptance of X-ray absorption spectroscopy (XAS) as a research tool in the environmental and geo-sciences. Independent of physical state (solid, liquid, gas), XAS analyses of metal(loid)s in complex environmental matrices over the past two decades have provided important information about speciation at environmentally relevant interfaces (e.g. solid-liquid) as well as in different media: plant tissues, rhizosphere, soils, sediments, ores, mineral process tailings, etc. Limited sample preparation requirements, the concomitant ability to preserve original physical and chemical states, and independence from crystallinity add to the advantages of using XAS in environmental investigations. Interpretations of XAS data are founded on sound physical and statistical models that can be applied to spectra of reference materials and mixed phases, respectively. For spectra collected directly from environmental matrices, abstract factor analysis and linear combination fitting provide the means to ascertain chemical, bonding, and crystalline states, and to extract quantitative information about their distribution within the data set. Through advances in optics, detectors, and data processing, X-ray fluorescence microprobes capable of focusing X-rays to micro- and nano-meter size have become competitive research venues for resolving the complexity of environmental samples at their inherent scale. The application of μ-XANES imaging, a new combinatorial approach of X-ray fluorescence spectrometry and XANES spectroscopy at the micron scale, is one of the latest technological advances allowing for lateral resolution of chemical states over wide areas due to vastly improved data processing and detector technology. Copyright © 2014. Published by Elsevier B.V.

  7. High sensitive X-ray films to detect electron showers in 100 GeV region

    NASA Technical Reports Server (NTRS)

    Taira, T.; Shirai, T.; Tateyama, N.; Torii, S.; Nishimura, J.; Fujii, M.; Yoshida, A.; Aizu, H.; Nomura, Y.; Kazuno, M.

    1985-01-01

    Nonscreen type X-ray films were used in emulsion chamber experiments to detect high energy showers in cosmic rays. Ranges of the detection threshold is from about 1 to 2 TeV depending on the exposure conditions. Different types of X-ray films and sheets i.e. high sensitive screen type X-ray films and luminescence sheets were tested. The threshold of the shower detection is found to be about 200 GeV, which is much lower than that of nonscreen type X-ray films. These films are useful to detect showers in the medium energy range, a few hundred GeV, of the cosmic ray electrons.

  8. X-ray fluorescence mapping of mercury on suspended mineral particles and diatoms in a contaminated freshwater system

    NASA Astrophysics Data System (ADS)

    Gu, B.; Mishra, B.; Miller, C.; Wang, W.; Lai, B.; Brooks, S. C.; Kemner, K. M.; Liang, L.

    2014-09-01

    Mercury (Hg) bioavailability and geochemical cycling is affected by its partitioning between the aqueous and particulate phases. We applied a synchrotron-based X-ray fluorescence (XRF) microprobe to visualize and quantify directly the spatial localization of Hg and its correlations with other elements of interest on suspended particles from a Hg-contaminated freshwater system. Up to 175 μg g-1 Hg is found on suspended particles, but less than 0.01% is in the form of methylmercury. Mercury is heterogeneously distributed among phytoplankton (e.g., diatoms) and mineral particles that are rich in iron oxides and natural organic matter (NOM). The diatom-bound Hg is mostly found on outer surfaces of the cells, suggesting passive sorption of Hg on diatoms. Our results indicate that localized sorption of Hg onto suspended particles, including diatoms and NOM-coated oxide minerals, may play an important role in affecting the partitioning, reactivity, and biogeochemical cycling of Hg in natural aquatic environments.

  9. X-ray fluorescence mapping of mercury on suspended mineral particles and diatoms in a contaminated freshwater system

    DOE PAGES

    Gu, Baohua; Mishra, Bhoopesh; Miller, Carrie L.; ...

    2014-01-01

    Mercury (Hg) bioavailability and geochemical cycling is affected by its partitioning between the aqueous and particulate phases. We applied a synchrotron-based X-ray fluorescence (XRF) microprobe to visualize and quantify directly the spatial localization of Hg and its correlations with other elements of interest on suspended particles from a Hg-contaminated freshwater system. Up to 175 μg g −1 Hg is found on suspended particles, but less than 0.01% is in the form of methylmercury. Mercury is heterogeneously distributed among phytoplankton (e.g., diatoms) and mineral particles that are rich in iron oxides and natural organic matter (NOM). The diatom-bound Hg is mostlymore » found on outer surfaces of the cells, suggesting passive sorption of Hg on diatoms. Our results indicate that localized sorption of Hg onto suspended particles, including diatoms and NOM-coated oxide minerals, may play an important role in affecting the partitioning, reactivity, and biogeochemical cycling of Hg in natural aquatic environments.« less

  10. Polymeric and Molecular Materials for Advanced Organic Electronics

    DTIC Science & Technology

    2014-10-20

    x - ray reflectivity, grazing incidence x - ray scattering, cyclic voltam- metry...6). ix These materials are characterized by AFM, conducting AFM, XPS, x - ray reflectivity (XRR), standing wave x - ray reflectivity (SWXRR), x - ray ...radiation hard - ness measurements, and quantum chemical computation of dielectric constants. Remark- ably, for semiconductors as diverse

  11. Improved performances of CIBER-X: a new tabletop laser-driven electron and x-ray source

    NASA Astrophysics Data System (ADS)

    Girardeau-Montaut, Jean-Pierre; Kiraly, Bela; Girardeau-Montaut, Claire

    2000-11-01

    We present the most recent data concerning the performances of the table-top laser driven electron and x-ray source developed in our laboratory. X-ray pulses are produced by a three-step process which consists of the photoelectron emission from a thin metallic photocathode illuminated by 16 ps duration laser pulse at 213 nm. The e-gun is a standard pierce diode electrode type, in which electrons are accelerated by a cw electric fields of 12 MV/m. The photoinjector produced a train of 90 - 100 keV electron pulses of approximately 1 nC and 40 A peak current at a repetition rate of 10 Hz. The electrons, transported outside the diode, are focused onto a target of thulium by magnetic fields produced by two electromagnetic coils to produce x-rays. Applications to low dose imagery of inert and living materials are also presented.

  12. AN OSCILLATOR CONFIGURATION FOR FULL REALIZATION OF HARD X-RAY FREE ELECTRON LASER*

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

    Kim, K.-J.; Kolodziej, T.; Lindberg, R. R.

    2017-06-01

    An x-ray free electron laser oscillator (XFELO) is feasible by employing an X-ray cavity with Bragg mirrors such as diamond crystals. An XFELO at the 5th harmonic frequency may be implemented at the LCLS II using its 4 GeV superconducting linac, producing stable, fully coherent, high-spectral-purity hard x-rays. In addition, its output can be a coherent seed to the LCLS amplifier for stable, high-power, femto-second x-ray pulses. We summarize the recent progress in various R&D efforts addressing critical issues for realizing an XFELO at LCLS II.

  13. In-Orbit Performance of the Digital Electronics for the X-Ray Microcalorimeter Onboard the Hitomi Satellite

    NASA Astrophysics Data System (ADS)

    Tsujimoto, M.; Tashiro, M. S.; Ishisaki, Y.; Yamada, S.; Seta, H.; Mitsuda, K.; Boyce, K. R.; Eckart, M. E.; Kilbourne, C. A.; Leutenegger, M. A.; Porter, F. S.; Kelley, R. L.

    2018-03-01

    The pulse shape processor is the onboard digital electronics unit of the X-ray microcalorimeter instrument—the soft X-ray spectrometer—onboard the Hitomi satellite. It processes X-ray events using the optimum filtering with limited resources. It was operated for 36 days in orbit continuously without issues and met the requirement of processing a 150 s^{-1} event rate during the observation of bright sources. Here, we present the results obtained in orbit, focusing on its performance as the onboard digital signal processing unit of an X-ray microcalorimeter.

  14. Normal incidence x-ray mirror for chemical microanalysis

    DOEpatents

    Carr, M.J.; Romig, A.D. Jr.

    1987-08-05

    An x-ray mirror for both electron column instruments and micro x-ray fluorescence instruments for making chemical, microanalysis comprises a non-planar mirror having, for example, a spherical reflecting surface for x-rays comprised of a predetermined number of alternating layers of high atomic number material and low atomic number material contiguously formed on a substrate and whose layers have a thickness which is a multiple of the wavelength being reflected. For electron column instruments, the wavelengths of interest lie above 1.5nm, while for x-ray fluorescence instruments, the range of interest is below 0.2nm. 4 figs.

  15. Temporal cross-correlation of x-ray free electron and optical lasers using soft x-ray pulse induced transient reflectivity.

    PubMed

    Krupin, O; Trigo, M; Schlotter, W F; Beye, M; Sorgenfrei, F; Turner, J J; Reis, D A; Gerken, N; Lee, S; Lee, W S; Hays, G; Acremann, Y; Abbey, B; Coffee, R; Messerschmidt, M; Hau-Riege, S P; Lapertot, G; Lüning, J; Heimann, P; Soufli, R; Fernández-Perea, M; Rowen, M; Holmes, M; Molodtsov, S L; Föhlisch, A; Wurth, W

    2012-05-07

    The recent development of x-ray free electron lasers providing coherent, femtosecond-long pulses of high brilliance and variable energy opens new areas of scientific research in a variety of disciplines such as physics, chemistry, and biology. Pump-probe experimental techniques which observe the temporal evolution of systems after optical or x-ray pulse excitation are one of the main experimental schemes currently in use for ultrafast studies. The key challenge in these experiments is to reliably achieve temporal and spatial overlap of the x-ray and optical pulses. Here we present measurements of the x-ray pulse induced transient change of optical reflectivity from a variety of materials covering the soft x-ray photon energy range from 500eV to 2000eV and outline the use of this technique to establish and characterize temporal synchronization of the optical-laser and FEL x-ray pulses.

  16. X-Ray Detector for 1 to 30 keV

    NASA Technical Reports Server (NTRS)

    Alcorn, G.; Jackson, J., Jr; Grant, P.; Marshall, F.

    1983-01-01

    Array of silicon X-ray detecting diodes measures photon energy and provides image of X-ray pattern. Regardless of thickness of new X-ray detector, depletion region extends through it. Impinging X-rays generate electrons in quantities proportional to X-ray energy. X-ray detector is mated to chargecoupled-device array for image generation and processing. Useful in industrial part inspection, pulsed-plasma research and medical application.

  17. Reflex Triode X-Ray Source Research on Gamble

    DTIC Science & Technology

    2007-06-01

    dosimeters ( TLDs ) located at the vacuum window (18-27 cm from the converter), near the pinhole camera and near the image plate. II. EXPERIMENTAL...MeV- electron beams to thin converters in order to optimize emission of sub-100- keV x-rays. Thin converters reduce self-absorption of low-energy...x-rays, but the beam electrons must pass many times through the converter for efficient x-ray production. The triode configuration was found to be

  18. Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

    DOE PAGES

    Kern, Jan; Yachandra, Vittal K.; Yano, Junko

    2015-09-02

    We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

  19. Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

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

    Kern, Jan; Yachandra, Vittal K.; Yano, Junko

    We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

  20. Experimental characterization of an ultra-fast Thomson scattering x-ray source with three-dimensional time and frequency-domain analysis

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

    Kuba, J; Slaughter, D R; Fittinghoff, D N

    We present a detailed comparison of the measured characteristics of Thomson backscattered x-rays produced at the PLEIADES (Picosecond Laser-Electron Interaction for the Dynamic Evaluation of Structures) facility at Lawrence Livermore National Laboratory to predicted results from a newly developed, fully three-dimensional time and frequency-domain code. Based on the relativistic differential cross section, this code has the capability to calculate time and space dependent spectra of the x-ray photons produced from linear Thomson scattering for both bandwidth-limited and chirped incident laser pulses. Spectral broadening of the scattered x-ray pulse resulting from the incident laser bandwidth, perpendicular wave vector components in themore » laser focus, and the transverse and longitudinal phase space of the electron beam are included. Electron beam energy, energy spread, and transverse phase space measurements of the electron beam at the interaction point are presented, and the corresponding predicted x-ray characteristics are determined. In addition, time-integrated measurements of the x-rays produced from the interaction are presented, and shown to agree well with the simulations.« less

  1. Mitigation of Hot Electrons from Laser-Plasma Instabilities in Laser-Generated X-Ray Sources

    NASA Astrophysics Data System (ADS)

    Fein, Jeffrey R.

    This thesis describes experiments to understand and mitigate energetic or "hot" electrons from laser-plasma instabilities (LPIs) in an effort to improve radiographic techniques using laser-generated x-ray sources. Initial experiments on the OMEGA-60 laser show evidence of an underlying background generated by x-rays with energies over 10 keV on radiographs using backlit pinhole radiography, whose source is consistent with hard x-rays from LPI-generated hot electrons. Mitigating this background can dramatically reduce uncertainties in measured object densities from radiographs and may be achieved by eliminating the target components in which LPIs are most likely to grow. Experiments were performed on the OMEGA-EP laser to study hot electron production from laser-plasma instabilities in high-Z plasmas relevant to laser-generated x-ray sources. Measurements of hard x-rays show a dramatic reduction in hot-electron energy going from low-Z CH to high-Z Au targets, in a manner that is consistent with steepening electron density profiles that were also measured. The profile-steepening, we infer, increased thresholds of LPIs and contributed to the reduced hot-electron production at higher Z. Possible mechanisms for generating hot electrons include the two-plasmon decay and stimulated Raman scattering instabilities driven by multiple laser beams. Radiation hydrodynamic simulations using the CRASH code predict that both of these instabilities were above threshold with linear threshold parameters that decreased with increasing Z due to steepening length-scales, as well as enhanced laser absorption and increased collisional and Landau damping of electron plasma waves. Another set of experiments were performed on the OMEGA-60 laser to test whether hard x-ray background could be mitigated in backlit pinhole imagers by controlling laser-plasma instabilities. Based on the results above, we hypothesized that LPIs and hot electrons that lead to hard x-ray background would be reduced by increasing the atomic number of the irradiated components in the pinhole imagers. Using higher-Z materials we demonstrate significant reduction in x-rays between 30-70 keV and 70% increase in the signal-to-background ratio. Based on this, a proposed backlighter and detector setup predicts a signal-to-background ratio of up to 4.5:1.

  2. Applications of RIGAKU Dmax Rapid II micro-X-ray diffractometer in the analysis of archaeological metal objects

    NASA Astrophysics Data System (ADS)

    Mozgai, Viktória; Szabó, Máté; Bajnóczi, Bernadett; Weiszburg, Tamás G.; Fórizs, István; Mráv, Zsolt; Tóth, Mária

    2017-04-01

    During material analysis of archaeological metal objects, especially their inlays or corrosion products, not only microstructure and chemical composition, but mineralogical composition is necessary to be determined. X-ray powder diffraction (XRD) is a widely-used method to specify the mineralogical composition. However, when sampling is not or limitedly allowed due to e.g. the high value of the object, the conventional XRD analysis can hardly be used. Laboratory micro-XRD instruments provide good alternatives, like the RIGAKU Dmax Rapid II micro-X-ray diffractometer, which is a unique combination of a MicroMax-003 third generation microfocus, sealed tube X-ray generator and a curved 'image plate' detector. With this instrument it is possible to measure as small as 10 µm area in diameter on the object. Here we present case studies for the application of the micro-XRD technique in the study of archaeological metal objects. In the first case niello inlay of a Late Roman silver augur staff was analysed. Due to the high value of the object, since it is the only piece known from the Roman Empire, only non-destructive analyses were allowed. To reconstruct the preparation of the niello, SEM-EDX analysis was performed on the niello inlays to characterise their chemical composition and microstructure. Two types of niello are present: a homogeneous, silver sulphide niello (acanthite) and an inhomogeneous silver-copper sulphide niello (exsolution of acanthite and jalpaite or jalpaite and stromeyerite). The micro-X-ray diffractometer was used to verify the mineralogical composition of the niello, supposed on the base of SEM results. In the second case corrosion products of a Late Roman copper cauldron with uncertain provenance were examined, since they may hold clues about the burial conditions (pH, Eh, etc.) of the object. A layer by layer analysis was performed in cross sections of small metal samples by using electron microprobe and micro-X-ray diffractometer. The results show two corrosion zones: 1) the original (internal) surface zone of the metallic copper object was replaced by copper(I) oxide (cuprite), while 2) basic copper(II) carbonate (malachite) was deposited (externally) on the original surface. In our view these two minerals were formed during long-time burial, and protected the cauldron from further corrosion. Rarely copper(I) chloride (nantokite), basic copper(II) trihydroxychloride (atacamite/paratacamite) and basic copper(II) sulphate (brochantite) were also identified in the two corrosion zones. Their uneven distribution on the cauldron and their known formation conditions indicate, that these latter mineral phases may be the results of active corrosion, started possibly after excavation.

  3. Calibration of high-dynamic-range, finite-resolution x-ray pulse-height spectrometers for extracting electron energy distribution data from the PFRC-2 device

    NASA Astrophysics Data System (ADS)

    Swanson, C.; Jandovitz, P.; Cohen, S. A.

    2017-10-01

    Knowledge of the full x-ray energy distribution function (XEDF) emitted from a plasma over a large dynamic range of energies can yield valuable insights about the electron energy distribution function (EEDF) of that plasma and the dynamic processes that create them. X-ray pulse height detectors such as Amptek's X-123 Fast SDD with Silicon Nitride window can detect x-rays in the range of 200eV to 100s of keV. However, extracting EEDF from this measurement requires precise knowledge of the detector's response function. This response function, including the energy scale calibration, the window transmission function, and the resolution function, can be measured directly. We describe measurements of this function from x-rays from a mono-energetic electron beam in a purpose-built gas-target x-ray tube. Large-Z effects such as line radiation, nuclear charge screening, and polarizational Bremsstrahlung are discussed.

  4. Electron microprobe study of lunar and planetary zoned plagioclase feldspars: An analytical and experimental study of zoning in plagioclase

    NASA Technical Reports Server (NTRS)

    Smith, R. K.; Lofgren, G. E.

    1982-01-01

    Natural and experimentally grown zoned plagioclase feldspars were examined by electron microprobe. The analyses revealed discontinuous, sector, and oscillary chemical zoning superimposed on continuous normal or reverse zoning trends. Postulated mechanisms for the origin of zoning are based on either physical changes external to the magma (P, T, H2O saturation) or kinetic changes internal to the magma (diffusion, supersaturation, growth rate). Comparison of microprobe data on natural zoned plagioclase with zoned plagioclase grown in controlled experiments show that it may be possible to distinguish zonal development resulting from physio-chemical changes to the bulk magma from local kinetic control on the growth of individual crystals.

  5. Crystal structure refinement and Mössbauer spectroscopy of an ordered, triclinic clinochlore

    USGS Publications Warehouse

    Smyth, Joseph R.; Dyar, M. Darby; May, Howard M.; Bricker, Owen P.; Acker, James G.

    1997-01-01

    The crystal structure of a natural, ordered IIb-4 triclinic clinochlore has been refined in space group C1¯ from 4282 unique X-ray intensity measurements of which 3833 are greater than 3 times the statistical counting error (3σ). Unit cell parameters are a = 5.3262(6) Å; b = 9.226(1) Å; c = 14.334(3) Å; α = 90.56(2)°; β = 97.47(2)°; and γ = 89.979(9)°, which represents the greatest deviation from monoclinic symmetry yet recorded for a triclinic chlorite. The final weighted R is 0.059 for reflections with I > 3σ and 0.064 for all reflections. The chemical formula is (Mg0.966Fe0.034)M1(Mg0.962Fe0.038)M22(Si2.96Al1.04)O10 (OH)2(Mg0.996Fe0.004)M32(Al0.841FeIII0.102Cr0.004Ti0.004)M4(OH)6, which is consistent with electron microprobe (EMP), wet chemical analyses, Mössbauer spectroscopy and X-ray structure refinement. The high degree of ordering of the divalent versus trivalent octahedral cations in the interlayer is noteworthy, with FeIII and Al in M4 and virtually no Fe in M3. In the 2:1 layer, M1 and M2 each contain similar amounts of Fe. The 2 tetrahedral sites have nearly identical mean oxygen distances and volumes, and thus show no evidence of long-range cation ordering.

  6. Mode-Locked Multichromatic X-Rays in a Seeded Free-Electron Laser for Single-Shot X-Ray Spectroscopy

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

    Xiang, Dao; Ding, Yuantao; Raubenheimer, Tor

    2012-05-10

    We present the promise of generating gigawatt mode-locked multichromatic x rays in a seeded free-electron laser (FEL). We show that, by using a laser to imprint periodic modulation in electron beam phase space, a single-frequency coherent seed can be amplified and further translated to a mode-locked multichromatic output in an FEL. With this configuration the FEL output consists of a train of mode-locked ultrashort pulses which span a wide frequency gap with a series of equally spaced sharp lines. These gigawatt multichromatic x rays may potentially allow one to explore the structure and dynamics of a large number of atomicmore » states simultaneously. The feasibility of generating mode-locked x rays ranging from carbon K edge ({approx}284 eV) to copper L{sub 3} edge ({approx}931 eV) is confirmed with numerical simulation using the realistic parameters of the linac coherent light source (LCLS) and LCLS-II. We anticipate that the mode-locked multichromatic x rays in FELs may open up new opportunities in x-ray spectroscopy (i.e. resonant inelastic x-ray scattering, time-resolved scattering and spectroscopy, etc.).« less

  7. X-ray Microprobe Investigations of Elemental Distributions and Concentrations at Mineral-Microbe Interfaces

    NASA Astrophysics Data System (ADS)

    Kemner, K. M.; Kelly, S. D.; O'Loughlin, E. J.; Lai, B.; Maser, J.; Cai, Z.; Londer, Y.; Schiffer, M.; Nealson, K.

    2003-12-01

    Understanding the fate of heavy-metal contaminants in the environment is of fundamental importance in the development and evaluation of effective remediation and sequestration strategies. Bacteria and the extracellular material associated with them are thought to play a key role in determining a contaminant's speciation and thus its mobility in the environment. Additionally, the metabolism and surface properties of bacteria can be quite different depending upon whether the bacteria exhibit a planktonic (free-floating) or biofilm (surface adhered) habit. The microenvironment at and adjacent to actively metabolizing cells also can be significantly different from the bulk environment. Thus, to understand the microscopic physical, geological, chemical, and biological interfaces that determine a contaminant's macroscopic fate, the spatial distribution and chemical speciation of contaminants and elements that are key to biological processes must be characterized at micron and submicron lengthscales for bacteria in both planktonic and adhered states. Hard x-ray microimaging is a powerful technique for the element-specific investigation of complex environmental samples at the needed micron and submicron resolution. An important advantage of these techniques results from the large penetration depth of hard x-rays in water. This advantage minimizes the requirements for sample preparation and allows the detailed study of hydrated samples. The objectives of the studies to be presented are (1) to determine the spatial distribution, concentration, and chemical speciation of metals at, in, and near bacteria and bacteria-geosurface interfaces, (2) to use this information to identify the metabolic processes occurring within the microbes, and (3) to identify the interactions occurring near these interfaces among the metals, mineral surfaces, and bacteria under a variety of conditions. We have used x-ray fluorescence microscopy to investigate the spatial distribution of 3d elements in Pseudomonas fluorescens cells in both planktonic and surface-adhered states. We have used x-ray fluorescence spectromicroscopy to investigate the chemical speciation and distribution of Cr that was introduced to these cells as Cr(VI). Additionally, we have used these techniques to identify the distribution of an over expressed cytochrome c7 in individual E. coli. Finally, we have used x-ray fluorescence microscopy to investigate Shewanella oneidensis MR-1 cells adhered to iron oxyhydroxide thin films. The zone plate used in these microscopy experiments produced a focused beam with a cross section (and hence spatial resolution) of 100-300 nanometers. Results from x-ray fluorescence imaging experiments indicate that the distribution of P, S, Cl, Ca, Fe, Ni, Cu, and Zn can define the location of the microbe. Additionally, quantitative elemental analysis of individual microbes identified significant changes in concentration of 3d transition elements depending on the age of the culture and the type of electron acceptor presented to the microbes. These results and a discussion of the use of this technique for identifying metabolic states of individual microbes within communities and the chemical speciation of metal contaminants at the mineral-microbe interface will be presented.

  8. Rat Phantom Depth Dose Studies in Electron, X-ray, Gamma-Ray, and Reactor Radiation Fields

    DTIC Science & Technology

    1986-12-01

    i©™D©/^ ^1[P@^T Rat phantom depth dose studies in electron , Xrayf gamma-ray, and reactor radiation fields M. Dooley D. M. Eagleson G. H. Zeman...energy electrons , bremsstrahlung, and mixed neutron/gamma radiation fields are sometimes used in radiobiological experiments employing rats. This report...have revealed differing sensitivities of experimental animals that have been exposed to cobalt-60 photons, high-energy electrons , high-energy X rays

  9. CORRELATION OF HARD X-RAY AND WHITE LIGHT EMISSION IN SOLAR FLARES

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

    Kuhar, Matej; Krucker, Säm; Battaglia, Marina

    A statistical study of the correlation between hard X-ray and white light emission in solar flares is performed in order to search for a link between flare-accelerated electrons and white light formation. We analyze 43 flares spanning GOES classes M and X using observations from the Reuven Ramaty High Energy Solar Spectroscopic Imager and Helioseismic and Magnetic Imager. We calculate X-ray fluxes at 30 keV and white light fluxes at 6173 Å summed over the hard X-ray flare ribbons with an integration time of 45 s around the peak hard-X ray time. We find a good correlation between hard X-raymore » fluxes and excess white light fluxes, with a highest correlation coefficient of 0.68 for photons with energy of 30 keV. Assuming the thick target model, a similar correlation is found between the deposited power by flare-accelerated electrons and the white light fluxes. The correlation coefficient is found to be largest for energy deposition by electrons above ∼50 keV. At higher electron energies the correlation decreases gradually while a rapid decrease is seen if the energy provided by low-energy electrons is added. This suggests that flare-accelerated electrons of energy ∼50 keV are the main source for white light production.« less

  10. Clusters in intense x-ray pulses

    NASA Astrophysics Data System (ADS)

    Bostedt, Christoph

    2012-06-01

    Free-electron lasers can deliver extremely intense, coherent x-ray flashes with femtosecond pulse length, opening the door for imaging single nanoscale objects in a single shot. All matter irradiated by these intense x-ray pulses, however, will be transformed into a highly-excited non-equilibrium plasma within femtoseconds. During the x-ray pulse complex electron dynamics and the onset of atomic disorder will be induced, leading to a time-varying sample. We have performed first experiments about x-ray laser pulse -- cluster interaction with a combined spectroscopy and imaging approach at both, the FLASH free electron laser in Hamburg (Germany) and the LCLS x-ray free-electron laser in Stanford (California). Atomic clusters are ideal for investigating the light - matter interaction because their size can be tuned from the molecular to the bulk regime, thus allowing to distinguish between intra and inter atomic processes. Imaging experiments with xenon clusters show power-density dependent changes in the scattering patterns. Modeling the scattering data indicates that the optical constants of the clusters change during the femtosecond pulse due to the transient creation of high charge states. The results show that ultra fast scattering is a promising approach to study transient states of matter on a femtosecond time scale. Coincident recording of time-of-flight spectra and scattering patterns allows the deconvolution of focal volume and particle size distribution effects. Single-shot single-particle experiments with keV x-rays reveal that for the highest power densities an highly excited and hot cluster plasma is formed for which recombination is suppressed. Time resolved infrared pump -- x-ray probe experiments have started. Here, the clusters are pumped into a nanoplasma state and their time evolution is probed with femtosecond x-ray scattering. The data show strong variations in the scattering patterns stemming from electronic reconfigurations in the cluster plasma. The results will be compared to theoretical predictions and discussed in light of current developments at free-electron laser sources.

  11. Photoluminescence studies on Cd(1-x)Zn(x)S:Mn2+ nanocrystals.

    PubMed

    Sethi, Ruchi; Kumar, Lokendra; Pandey, A C

    2009-09-01

    Highly monodispersed, undoped and doped with Mn2+, binary and ternary (CdS, ZnS, Cd(1-x)Zn(x)S) compound semiconductor nanocrystals have been synthesized by co-precipitation method using citric acid as a stabilizer. As prepared sample are characterized by X-ray diffraction, Small angle X-ray scattering, Transmission electron microscope, Optical absorption and Photoluminescence spectroscopy, for their optical and structural properties. X-ray diffraction, Small angle X-ray scattering and Transmission electron microscope results confirm the preparation of monodispersed nanocrystals. Photoluminescence studies show a significant blue shift in the wavelength with an increasing concentration of Zn in alloy nanocrystals.

  12. A Flash X-Ray Facility for the Naval Postgraduate School

    DTIC Science & Technology

    1985-06-01

    ionizing radiation, *• NPS has had active programs with a Van de Graaff generator, a reactor, radioactive sources, X-ray machines and a linear electron ...interaction of radiation with matter and with coherent radiation. Currently the most active program is at the linear electron accelerator which over...twenty years has produced some 75 theses. The flash X-ray machine was obtained to expan-i and complement the capabilities of the linear electron

  13. The Fate of ZnO Nanoparticles Administered to Human Bronchial Epithelial Cells

    PubMed Central

    Gilbert, Benjamin; Fakra, Sirine C.; Xia, Tian; Pokhrel, Suman; Mädler, Lutz; Nel, André E.

    2014-01-01

    A particular challenge for nanotoxicology is the evaluation of the biological fate and toxicity of nanomaterials that dissolve in aqueous fluids. Zinc oxide nanomaterials are of particular concern because dissolution leads to release of the toxic divalent zinc ion. Although dissolved zinc ions have been implicated in ZnO cytotoxicity, direct identification of the chemical form of zinc taken up by cells exposed to ZnO nanoparticles, and its intracellular fate, has not yet been achieved. We combined high resolution X-ray spectromicroscopy and high elemental sensitivity X-ray microprobe analyses to determine the fate of ZnO and less soluble iron-doped ZnO nanoparticles following exposure to cultures of human bronchial epithelial cells, BEAS-2B. We complemented two-dimensional X-ray imaging methods with atomic force microscopy of cell surfaces to distinguish between nanoparticles that were transported inside the cells from those that adhered to the cell exterior. The data suggest cellular uptake of ZnO nanoparticles is a mechanism of zinc accumulation in cells. Following uptake, ZnO nanoparticles dissolved completely generating intracellular Zn2+ complexed by molecular ligands. These results corroborate a model for ZnO nanoparticle toxicity that is based on nanoparticle uptake followed by intracellular dissolution. PMID:22646753

  14. Modeling the gain of inner-shell X-ray laser transitions in neon, argon, and copper driven by X-ray free electron laser radiation using photo-ionization and photo-excitation processes

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

    Nilsen, Joseph

    2015-12-16

    Using an X-ray free electron laser (XFEL) at 960 eV to photo-ionize the 1s electron in neutral neon followed by lasing on the 2p-1s transition in singly-ionized neon, an inner-shell X-ray laser was demonstrated at 849 eV in singly-ionized neon gas several years ago. It took decades to demonstrate this scheme, because it required a very strong X-ray source that could photo-ionize the 1s (K shell) electron in neon on a timescale comparable to the intrinsic Auger lifetime in neon of 2 fs. In this paper, we model the neon inner shell X-ray laser under similar conditions to those usedmore » in the XFEL experiments at the SLAC Linac Coherent Light Source (LCLS), and show how we can improve the efficiency of the neon laser and reduce the drive requirements by tuning the XFEL to the 1s-3p transition in neutral neon in order to create gain on the 2p-1s line in neutral neon. We also show how the XFEL could be used to photo-ionize L-shell electrons to drive gain on n = 3–2 transitions in singly-ionized Ar and Cu plasmas. Furthermore, these bright, coherent, and monochromatic X-ray lasers may prove very useful for doing high-resolution spectroscopy and for studying non-linear process in the X-ray regime.« less

  15. Low-energy d-d excitations in MnO studied by resonant x-ray fluorescence spectroscopy

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

    Butorin, S.M.; Guo, J.; Magnuson, M.

    1997-04-01

    Resonant soft X-ray emission spectroscopy has been demonstrated to possess interesting abilities for studies of electronic structure in various systems, such as symmetry probing, alignment and polarization dependence, sensitivity to channel interference, etc. In the present abstract the authors focus on the feasibility of resonant soft X-ray emission to probe low energy excitations by means of resonant electronic X-ray Raman scattering. Resonant X-ray emission can be regarded as an inelastic scattering process where a system in the ground state is transferred to a low excited state via a virtual core excitation. The energy closeness to a core excitation of themore » exciting radiation enhances the (generally) low probability for inelastic scattering at these wavelengths. Therefore soft X-ray emission spectroscopy (in resonant electronic Raman mode) can be used to study low energy d-d excitations in transition metal systems. The involvement of the intermediate core state allows one to use the selection rules of X-ray emission, and the appearance of the elastically scattered line in the spectra provides the reference to the ground state.« less

  16. Construction of a magnetic bottle spectrometer and its application to pulse duration measurement of X-ray laser using a pump-probe method

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

    Namba, S., E-mail: namba@hiroshima-u.ac.jp; Hasegawa, N.; Kishimoto, M.

    To characterize the temporal evolution of ultrashort X-ray pulses emitted by laser plasmas using a pump-probe method, a magnetic bottle time-of-flight electron spectrometer is constructed. The design is determined by numerical calculations of a mirror magnetic field and of the electron trajectory in a flight tube. The performance of the spectrometer is characterized by measuring the electron spectra of xenon atoms irradiated with a laser-driven plasma X-ray pulse. In addition, two-color above-threshold ionization (ATI) experiment is conducted for measurement of the X-ray laser pulse duration, in which xenon atoms are simultaneously irradiated with an X-ray laser pump and an IRmore » laser probe. The correlation in the intensity of the sideband spectra of the 4d inner-shell photoelectrons and in the time delay of the two laser pulses yields an X-ray pulse width of 5.7 ps, in good agreement with the value obtained using an X-ray streak camera.« less

  17. The Focusing Optics X-ray Solar Imager (FOXSI): Instrument and First Flight

    NASA Astrophysics Data System (ADS)

    Glesener, Lindsay; Christe, S.; Ishikawa, S.; Ramsey, B.; Takahashi, T.; Saito, S.; Lin, R. P.; Krucker, S.; FOXSI Team

    2013-04-01

    Understanding electron acceleration in solar flares requires hard X-ray studies with greater sensitivity and dynamic range than are available with current solar hard X-ray observers (i.e. the RHESSI spacecraft). Both these capabilities can be advanced by the use of direct focusing optics instead of the indirect Fourier methods of current and previous generations. The Focusing Optics X-ray Solar Imager (FOXSI) sounding rocket payload demonstrates the feasibility and usefulness of hard X-ray focusing optics for solar observation. FOXSI flew for the first time on 2012 November 2, producing images and spectra of a microflare and performing a search for nonthermal X-rays from the quiet Sun. Such measurements are important for characterizing the impact of small "nanoflares" on the solar coronal heating problem. A spaceborne solar observer featuring similar optics could make detailed observations of hard X-rays from flare-accelerated electrons, identifying and characterizing particle acceleration sites and mapping out paths of energetic electrons as they leave these sites and propagate throughout the solar corona. Solar observations from NuSTAR are also expected to be an important step in this direction.

  18. Total rate imaging with x-rays (TRIX)--a simple method of forming a non-projection x-ray image in the SEM using an energy dispersive detector and its application to biological specimens.

    PubMed

    Ingram, P; Shelburne, J D

    1980-01-01

    X-ray images can be formed in a conventional scanning electron microscope equipped with a Si(Li) energy dispersive spectrometer. All the x-ray events generated in the electron beam scanning process are synchronously displayed in the same manner as for dot maps. The quasi-digital image formed using Total Rate Imaging with X-rays (TRIX) exhibits good gray scale contrast and is dependent on topography, orientation and atomic number. Although this latter dependence is complex, it has been found useful in locating several types of inclusions in lung tissue (silicosis), human alveolar macrophages and cigarette smoke condensate. This is because of the greater depth of penetration of x-rays than backscattered electrons (BSE) usually used for such localizations in a matrix, and the negligible sensitivity of the Si(Li) detector to x-rays from an organic biological matrix. The optimum procedure is to use a combination of TRIX and BSE to investigate such specimens.

  19. High-resolution multi-MeV x-ray radiography using relativistic laser-solid interaction

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

    Courtois, C.; Compant La Fontaine, A.; Barbotin, M.

    2011-02-15

    When high intensity ({>=}10{sup 19} W cm{sup -2}) laser light interacts with matter, multi-MeV electrons are produced. These electrons can be utilized to generate a MeV bremsstrahlung x-ray emission spectrum as they propagate into a high-Z solid target positioned behind the interaction area. The short duration (<10 ps) and the small diameter (<500 {mu}m) of the x-ray pulse combined with the MeV x-ray spectrum offers an interesting alternative to conventional bremsstrahlung x-ray sources based on an electron accelerator used to radiograph dense, rapidly moving objects. In experiments at the Omega EP laser, a multi-MeV x-ray source is characterized consistently withmore » number of independent diagnostics. An unfiltered x-ray dose of approximately 2 rad in air at 1 m and a source diameter of less than 350 {mu}m are inferred. Radiography of a complex and high area density (up to 61 g/cm{sup 2}) object is then performed with few hundred microns spatial resolution.« less

  20. Surface applicator of a miniature X-ray tube for superficial electronic brachytherapy of skin cancer.

    PubMed

    Kim, Hyun Nam; Lee, Ju Hyuk; Park, Han Beom; Kim, Hyun Jin; Cho, Sung Oh

    2018-01-01

    We designed and fabricated a surface applicator of a novel carbon nanotube (CNT)-based miniature X-ray tube for the use in superficial electronic brachytherapy of skin cancer. To investigate the effectiveness of the surface applicator, the performance of the applicator was numerically and experimentally analyzed. The surface applicator consists of a graphite flattening filter and an X-ray shield. A Monte Carlo radiation transport code, MCNP6, was used to optimize the geometries of both the flattening filter and the shield so that X-rays are generated uniformly over the desired region. The performance of the graphite filter was compared with that of conventional aluminum (Al) filters of different geometries using the numerical simulations. After fabricating a surface applicator, the X-ray spatial distribution was measured to evaluate the performance of the applicator. The graphite filter shows better spatial dose uniformity and less dose distortion than Al filters. Moreover, graphite allows easy fabrication of the flattening filter due to its low X-ray attenuation property, which is particularly important for low-energy electronic brachytherapy. The applicator also shows that no further X-ray shielding is required for the application because unwanted X-rays are completely protected. As a result, highly uniform X-ray dose distribution was achieved from the miniature X-ray tube mounted with the surface applicators. The measured values of both flatness and symmetry were less than 5% and the measured penumbra values were less than 1 mm. All these values satisfy the currently accepted tolerance criteria for radiation therapy. The surface applicator exhibits sufficient performance capability for their application in electronic brachytherapy of skin cancers. © 2017 American Association of Physicists in Medicine.

  1. Resonant inelastic soft x-ray scattering of CdS: a two-dimensional electronic structure map approach

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

    Weinhardt, L.; Fuchs, O.; Fleszar, A.

    2008-09-24

    Resonant inelastic x-ray scattering (RIXS) with soft x-rays is uniquely suited to study the elec-tronic structure of a variety of materials, but is currently limited by low (fluorescence yield) count rates. This limitation is overcome with a new high-transmission spectrometer that allows to measure soft x-ray RIXS"maps." The S L2,3 RIXS map of CdS is discussed and compared with density functional calculations. The map allows the extraction of decay channel-specific"absorp-tion spectra," giving detailed insight into the wave functions of occupied and unoccupied elec-tronic states.

  2. Echo-Enabled X-Ray Vortex Generation

    NASA Astrophysics Data System (ADS)

    Hemsing, E.; Marinelli, A.

    2012-11-01

    A technique to generate high-brightness electromagnetic vortices with tunable topological charge at extreme ultraviolet and x-ray wavelengths is described. Based on a modified version of echo-enabled harmonic generation for free-electron lasers, the technique uses two lasers and two chicanes to produce high-harmonic microbunching of a relativistic electron beam with a corkscrew distribution that matches the instantaneous helical phase structure of the x-ray vortex. The strongly correlated electron distribution emerges from an efficient three-dimensional recoherence effect in the echo-enabled harmonic generation transport line and can emit fully coherent vortices in a downstream radiator for access to new research in x-ray science.

  3. Calibration of a time-resolved hard-x-ray detector using radioactive sources

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

    Stoeckl, C., E-mail: csto@lle.rochester.edu; Theobald, W.; Regan, S. P.

    A four-channel, time-resolved, hard x-ray detector (HXRD) has been operating at the Laboratory for Laser Energetics for more than a decade. The slope temperature of the hot-electron population in direct-drive inertial confinement fusion experiments is inferred by recording the hard x-ray radiation generated in the interaction of the electrons with the target. Measuring the energy deposited by hot electrons requires an absolute calibration of the hard x-ray detector. A novel method to obtain an absolute calibration of the HXRD using single photons from radioactive sources was developed, which uses a thermoelectrically cooled, low-noise, charge-sensitive amplifier.

  4. Valence-electron configuration of Fe, Cr, and Ni in binary and ternary alloys from Kβ -to- Kα x-ray intensity ratios

    NASA Astrophysics Data System (ADS)

    Han, I.; Demir, L.

    2009-11-01

    Kβ -to- Kα x-ray intensity ratios of Fe, Cr, and Ni have been measured in pure metals and in alloys of FexNi1-x ( x=0.8 , 0.7, 0.6, 0.5, 0.4, 0.3, and 0.2), NixCr1-x ( x=0.8 , 0.6, 0.5, 0.4, and 0.2), FexCr1-x ( x=0.9 , 0.7, and 0.5), and FexCryNi1-(x+y) ( x=0.7-y=0.1 , x=0.5-y=0.2 , x=0.4-y=0.3 , x=0.3-y=0.3 , x=0.2-y=0.2 , and x=0.1-y=0.2 ) following excitation by 22.69 keV x rays from a 10 mCi C109d radioactive point source. The valence-electron configurations of these metals were determined by corporation of measured Kβ -to- Kα x-ray intensity ratios with the results of multiconfiguration Dirac-Fock calculation for various valence-electron configurations. Valence-electron configurations of 3d transition metals in alloys indicate significant differences with respect to the pure metals. Our analysis indicates that these differences arise from delocalization and/or charge transfer phenomena in alloys. Namely, the observed change of the valence-electron configurations of metals in alloys can be explained with the transfer of 3d electrons from one element to the other element and/or the rearrangement of electrons between 3d and 4s,4p states of individual metal atoms.

  5. Deducing Electron Properties from Hard X-Ray Observations

    NASA Technical Reports Server (NTRS)

    Kontar, E. P.; Brown, J. C.; Emslie, A. G.; Hajdas, W.; Holman, G. D.; Hurford, G. J.; Kasparova, J.; Mallik, P. C. V.; Massone, A. M.; McConnell, M. L.; hide

    2011-01-01

    X-radiation from energetic electrons is the prime diagnostic of flare-accelerated electrons. The observed X-ray flux (and polarization state) is fundamentally a convolution of the cross-section for the hard X-ray emission process(es) in question with the electron distribution function, which is in turn a function of energy, direction, spatial location and time. To address the problems of particle propagation and acceleration one needs to infer as much information as possible on this electron distribution function, through a deconvolution of this fundamental relationship. This review presents recent progress toward this goal using spectroscopic, imaging and polarization measurements, primarily from the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI). Previous conclusions regarding the energy, angular (pitch angle) and spatial distributions of energetic electrons in solar flares are critically reviewed. We discuss the role and the observational evidence of several radiation processes: free-free electron-ion, free-free electron-electron, free-bound electron-ion, photoelectric absorption and Compton backscatter (albedo), using both spectroscopic and imaging techniques. This unprecedented quality of data allows for the first time inference of the angular distributions of the X-ray-emitting electrons and improved model-independent inference of electron energy spectra and emission measures of thermal plasma. Moreover, imaging spectroscopy has revealed hitherto unknown details of solar flare morphology and detailed spectroscopy of coronal, footpoint and extended sources in flaring regions. Additional attempts to measure hard X-ray polarization were not sufficient to put constraints on the degree of anisotropy of electrons, but point to the importance of obtaining good quality polarization data in the future.

  6. X-ray compass for determining device orientation

    DOEpatents

    Da Silva, Luiz B.; Matthews, Dennis L.; Fitch, Joseph P.; Everett, Matthew J.; Colston, Billy W.; Stone, Gary F.

    1999-01-01

    An apparatus and method for determining the orientation of a device with respect to an x-ray source. In one embodiment, the present invention is coupled to a medical device in order to determine the rotational orientation of the medical device with respect to the x-ray source. In such an embodiment, the present invention is comprised of a scintillator portion which is adapted to emit photons upon the absorption of x-rays emitted from the x-ray source. An x-ray blocking portion is coupled to the scintillator portion. The x-ray blocking portion is disposed so as to vary the quantity of x-rays which penetrate the scintillator portion based upon the particular rotational orientation of the medical device with respect to the x-ray source. A photon transport mechanism is also coupled to the scintillator portion. The photon transport mechanism is adapted to pass the photons emitted from the scintillator portion to an electronics portion. By analyzing the quantity of the photons, the electronics portion determines the rotational orientation of the medical device with respect to the x-ray source.

  7. X-ray compass for determining device orientation

    DOEpatents

    Da Silva, L.B.; Matthews, D.L.; Fitch, J.P.; Everett, M.J.; Colston, B.W.; Stone, G.F.

    1999-06-15

    An apparatus and method for determining the orientation of a device with respect to an x-ray source are disclosed. In one embodiment, the present invention is coupled to a medical device in order to determine the rotational orientation of the medical device with respect to the x-ray source. In such an embodiment, the present invention is comprised of a scintillator portion which is adapted to emit photons upon the absorption of x-rays emitted from the x-ray source. An x-ray blocking portion is coupled to the scintillator portion. The x-ray blocking portion is disposed so as to vary the quantity of x-rays which penetrate the scintillator portion based upon the particular rotational orientation of the medical device with respect to the x-ray source. A photon transport mechanism is also coupled to the scintillator portion. The photon transport mechanism is adapted to pass the photons emitted from the scintillator portion to an electronics portion. By analyzing the quantity of the photons, the electronics portion determines the rotational orientation of the medical device with respect to the x-ray source. 25 figs.

  8. Elucidating the Wavelength Dependence of Phonon Scattering in Nanoparticle-Matrix Composites using Phonon Spectroscopy

    DTIC Science & Technology

    2016-07-11

    composites with x - ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Rutherford backscattering spectroscopy...RBS), particle-induced x - ray emission (PIXE), and energy dispersive x - ray spectroscopy (EDX). This work complements earlier works on CdSe...sample shows only In2Se3 and CdIn2Se4 XRD peaks (Figure 1.4e), it is stoichiometrically   Figure 1.4. X - ray diffraction patterns of (a) γ-In2Se3

  9. 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

  10. Electronic structure of the organic semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from soft x-ray spectroscopies and density functional theory calculations.

    PubMed

    DeMasi, A; Piper, L F J; Zhang, Y; Reid, I; Wang, S; Smith, K E; Downes, J E; Peltekis, N; McGuinness, C; Matsuura, A

    2008-12-14

    The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq(3)) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq(3), and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studies and the present data reveal the presence of clear photon-induced damage in the former.

  11. Stimulated Electronic X-Ray Raman Scattering

    NASA Astrophysics Data System (ADS)

    Weninger, Clemens; Purvis, Michael; Ryan, Duncan; London, Richard A.; Bozek, John D.; Bostedt, Christoph; Graf, Alexander; Brown, Gregory; Rocca, Jorge J.; Rohringer, Nina

    2013-12-01

    We demonstrate strong stimulated inelastic x-ray scattering by resonantly exciting a dense gas target of neon with femtosecond, high-intensity x-ray pulses from an x-ray free-electron laser (XFEL). A small number of lower energy XFEL seed photons drive an avalanche of stimulated resonant inelastic x-ray scattering processes that amplify the Raman scattering signal by several orders of magnitude until it reaches saturation. Despite the large overall spectral width, the internal spiky structure of the XFEL spectrum determines the energy resolution of the scattering process in a statistical sense. This is demonstrated by observing a stochastic line shift of the inelastically scattered x-ray radiation. In conjunction with statistical methods, XFELs can be used for stimulated resonant inelastic x-ray scattering, with spectral resolution smaller than the natural width of the core-excited, intermediate state.

  12. Katherine E. Weimer Award: X-ray light sources from laser-plasma and laser-electron interaction: development and applications

    NASA Astrophysics Data System (ADS)

    Albert, Felicie

    2017-10-01

    Bright sources of x-rays, such as synchrotrons and x-ray free electron lasers (XFEL) are transformational tools for many fields of science. They are used for biology, material science, medicine, or industry. Such sources rely on conventional particle accelerators, where electrons are accelerated to gigaelectronvolts (GeV) energies. The accelerated particles are wiggled in magnetic structures to emit x-ray radiation that is commonly used for molecular crystallography, fluorescence studies, chemical analysis, medical imaging, and many other applications. One of the drawbacks of these machines is their size and cost, because electric field gradients are limited to about 100 V/M in conventional accelerators. Particle acceleration in laser-driven plasmas is an alternative to generate x-rays via betatron emission, Compton scattering, or bremsstrahlung. A plasma can sustain electrical fields many orders of magnitude higher than that in conventional radiofrequency accelerator structures. When short, intense laser pulses are focused into a gas, it produces electron plasma waves in which electrons can be trapped and accelerated to GeV energies. X-ray sources, driven by electrons from laser-wakefield acceleration, have unique properties that are analogous to synchrotron radiation, with a 1000-fold shorter pulse. An important use of x-rays from laser plasma accelerators is in High Energy Density (HED) science, which requires laser and XFEL facilities to create in the laboratory extreme conditions of temperatures and pressures that are usually found in the interiors of stars and planets. To diagnose such extreme states of matter, the development of efficient, versatile and fast (sub-picosecond scale) x-ray probes has become essential. In these experiments, x-ray photons can pass through dense material, and absorption of the x-rays can be directly measured, via spectroscopy or imaging, to inform scientists about the temperature and density of the targets being studied. Performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under contract DE-AC52-07NA27344, supported by the LLNL LDRD program (16ERD024), and by the DOE Office Science Early Career Research Program (SCW1575).

  13. An adjustable short-focal length, high-gradient PMQ electron-beam final-focus system for the PLEIADES ultra-fast x-ray Thomson source

    NASA Astrophysics Data System (ADS)

    Lim, Jae-Ku

    In the span of a 100 year since the discovery of first x-rays by Roentgen that won him the first Nobel prize in physics, several types of radiation sources have been developed. Currently, radiations at extremely short wavelengths have only been accessed at synchrotron radiation sources. However, the current 3rd generation synchrotron sources can only produce x-rays of energy up to 60 keV and pulse lengths of several picoseconds long. But needs for shorter wavelength and shorter pulse duration radiations demanded by scientists to understand the nature of matter at atomic/molecular scale initiated the new scientific research for the production of sub-picosecond, hard x-rays. At the Lawrence Livermore National Laboratory, a Thomson x-ray source in the backscattering mode---a head-on collision between a high intensity Ti:Sapphire Chirped Pulse Amplification laser and a relativistic electron beam---called the PLEIADES (Picosecond Laser-Electron Inter-Action for the Dynamical Evaluation of Structures) laboratory has been developed. Early works demonstrated the production of quasi-monochromatic, femto-second long, hard x-rays. Initially reported x-ray flux was in the low range of 105--10 6 photons per shot. During the early stage of PLEIADES experiments, 15 T/m electromagnet final focusing quadrupoles (in a triplet lattice configuration) were employed to focus the beam to a 40-50 mum spot-size. A larger focal spot-size beam has a low-density of electron particles available at the interaction with incident photons, which leads to a low scattering probability. The current dissertation shows that by employing a 560 T/m PMQ (Permanent-Magnet Quadrupole) final focus system, an electron beam as small as 10-20 mum can be achieved. The implementation of this final focus system demonstrated the improvement of the total x-ray flux by two orders of magnitude. The PMQ final focus system also produced small electron beams consistently over 30-100 MeV electron beam energy, which enabled the production of x-ray energy over 40-140 keV. In this dissertation, the PLEIADES Thomson x-ray facility will be described in detail includes the 100 MeV linac and the FALCON laser system. Later, we will discuss the design, construction and implementation of the PMQ final focus system in the beamline. The measurement of electron beam parameters before and after the final focus system will be presented. The beam measurements at the interaction region were accomplished with the use of both OTR (Optical Transition Radiation) imaged by a CCD camera and the fast streak camera for respective spatial and temporal alignments. The theoretical analysis in "real beam" effects and spacetime beam jitter effects will be given to help understand the observations. A 3D simulation tool developed for x-ray data analysis was used to provide direct comparisons with the x-ray flux, spectrum distribution and transverse x-ray profile.

  14. High flux, narrow bandwidth compton light sources via extended laser-electron interactions

    DOEpatents

    Barty, V P

    2015-01-13

    New configurations of lasers and electron beams efficiently and robustly produce high flux beams of bright, tunable, polarized quasi-monoenergetic x-rays and gamma-rays via laser-Compton scattering. Specifically, the use of long-duration, pulsed lasers and closely-spaced, low-charge and low emittance bunches of electron beams increase the spectral flux of the Compton-scattered x-rays and gamma rays, increase efficiency of the laser-electron interaction and significantly reduce the overall complexity of Compton based light sources.

  15. Calculating the X-Ray Fluorescence from the Planet Mercury Due to High-Energy Electrons

    NASA Technical Reports Server (NTRS)

    Burbine, T. H.; Trombka, J. I.; Bergstrom, P. M., Jr.; Christon, S. P.

    2005-01-01

    The least-studied terrestrial planet is Mercury due to its proximity to the Sun, which makes telescopic observations and spacecraft encounters difficult. Our lack of knowledge about Mercury should change in the near future due to the recent launching of MESSENGER, a Mercury orbiter. Another mission (BepiColombo) is currently being planned. The x-ray spectrometer on MESSENGER (and planned for BepiColombo) can characterize the elemental composition of a planetary surface by measuring emitted fluorescent x-rays. If electrons are ejected from an atom s inner shell by interaction with energetic particles such as photons, electrons, or ions, electrons from an outer shell can transfer to the inner shell. Characteristic x-rays are then emitted with energies that are the difference between the binding energy of the ion in its excited state and that of the ion in its ground state. Because each element has a unique set of energy levels, each element emits x-rays at a unique set of energies. Electrons and ions usually do not have the needed flux at high energies to cause significant x-ray fluorescence on most planetary bodies. This is not the case for Mercury where high-energy particles were detected during the Mariner 10 flybys. Mercury has an intrinsic magnetic field that deflects the solar wind, resulting in a bow shock in the solar wind and a magnetospheric cavity. Electrons and ions accelerated in the magnetosphere tend to follow its magnetic field lines and can impact the surface on Mercury s dark side Modeling has been done to determine if x-ray fluorescence resulting from the impact of high-energy electrons accelerated in Mercury's magnetosphere can be detected by MESSENGER. Our goal is to understand how much bulk chemical information can be obtained from x-ray fluorescence measurements on the dark side of Mercury.

  16. Advanced X-Ray Sources Ensure Safe Environments

    NASA Technical Reports Server (NTRS)

    2008-01-01

    Ames Research Center awarded inXitu Inc. (formerly Microwave Power Technology), of Mountain View, California, an SBIR contract to develop a new design of electron optics for forming and focusing electron beams that is applicable to a broad class of vacuum electron devices. This technology offers an inherently rugged and more efficient X-ray source for material analysis; a compact and rugged X-ray source for smaller rovers on future Mars missions; and electron beam sources to reduce undesirable emissions from small, widely distributed pollution sources; and remediation of polluted sites.

  17. Talbot-Lau x-ray deflectometry phase-retrieval methods for electron density diagnostics in high-energy density experiments.

    PubMed

    Valdivia, Maria Pia; Stutman, Dan; Stoeckl, Christian; Mileham, Chad; Begishev, Ildar A; Bromage, Jake; Regan, Sean P

    2018-01-10

    Talbot-Lau x-ray interferometry uses incoherent x-ray sources to measure refraction index changes in matter. These measurements can provide accurate electron density mapping through phase retrieval. An adaptation of the interferometer has been developed in order to meet the specific requirements of high-energy density experiments. This adaptation is known as a moiré deflectometer, which allows for single-shot capabilities in the form of interferometric fringe patterns. The moiré x-ray deflectometry technique requires a set of object and reference images in order to provide electron density maps, which can be costly in the high-energy density environment. In particular, synthetic reference phase images obtained ex situ through a phase-scan procedure, can provide a feasible solution. To test this procedure, an object phase map was retrieved from a single-shot moiré image obtained from a plasma-produced x-ray source. A reference phase map was then obtained from phase-stepping measurements using a continuous x-ray tube source in a small laboratory setting. The two phase maps were used to retrieve an electron density map. A comparison of the moiré and phase-stepping phase-retrieval methods was performed to evaluate single-exposure plasma electron density mapping for high-energy density and other transient plasma experiments. It was found that a combination of phase-retrieval methods can deliver accurate refraction angle mapping. Once x-ray backlighter quality is optimized, the ex situ method is expected to deliver electron density mapping with improved resolution. The steps necessary for improved diagnostic performance are discussed.

  18. Calculation of x-ray spectra emerging from an x-ray tube. Part I. electron penetration characteristics in x-ray targets.

    PubMed

    Poludniowski, Gavin G; Evans, Philip M

    2007-06-01

    The penetration characteristics of electron beams into x-ray targets are investigated for incident electron kinetic energies in the range 50-150 keV. The frequency densities of electrons penetrating to a depth x in a target, with a fraction of initial kinetic energy, u, are calculated using Monte Carlo methods for beam energies of 50, 80, 100, 120 and 150 keV in a tungsten target. The frequency densities for 100 keV electrons in Al, Mo and Re targets are also calculated. A mixture of simple modeling with equations and interpolation from data is used to generalize the calculations in tungsten. Where possible, parameters derived from the Monte Carlo data are compared to experimental measurements. Previous electron transport approximations in the semiempirical models of other authors are discussed and related to this work. In particular, the crudity of the use of the Thomson-Whiddington law to describe electron penetration and energy loss is highlighted. The results presented here may be used towards calculating the target self-attenuation correction for bremsstrahlung photons emitted within a tungsten target.

  19. Backscatter of hard X-rays in the solar atmosphere. [Calculating the reflectance of solar x ray emission

    NASA Technical Reports Server (NTRS)

    Bai, T.; Ramaty, R.

    1977-01-01

    The solar photosphere backscatters a substantial fraction of the hard X rays from solar flares incident upon it. This reflection was studied using a Monte Carlo simulation which takes into account Compton scattering and photo-electric absorption. Both isotropic and anisotropic X ray sources are considered. The bremsstrahlung from an anisotropic distribution of electrons are evaluated. By taking the reflection into account, the inconsistency is removed between recent observational data regarding the center-to-limb variation of solar X ray emission and the predictions of models in which accelerated electrons are moving down toward the photosphere.

  20. Fluorescence imaging of reactive oxygen species by confocal laser scanning microscopy for track analysis of synchrotron X-ray photoelectric nanoradiator dose: X-ray pump-optical probe.

    PubMed

    Jeon, Jae Kun; Han, Sung Mi; Kim, Jong Ki

    2016-09-01

    Bursts of emissions of low-energy electrons, including interatomic Coulomb decay electrons and Auger electrons (0-1000 eV), as well as X-ray fluorescence produced by irradiation of large-Z element nanoparticles by either X-ray photons or high-energy ion beams, is referred to as the nanoradiator effect. In therapeutic applications, this effect can damage pathological tissues that selectively take up the nanoparticles. Herein, a new nanoradiator dosimetry method is presented that uses probes for reactive oxygen species (ROS) incorporated into three-dimensional gels, on which macrophages containing iron oxide nanoparticles (IONs) are attached. This method, together with site-specific irradiation of the intracellular nanoparticles from a microbeam of polychromatic synchrotron X-rays (5-14 keV), measures the range and distribution of OH radicals produced by X-ray emission or superoxide anions ({\\rm{O}}_2^-) produced by low-energy electrons. The measurements are based on confocal laser scanning of the fluorescence of the hydroxyl radical probe 2-[6-(4'-amino)phenoxy-3H-xanthen-3-on-9-yl] benzoic acid (APF) or the superoxide probe hydroethidine-dihydroethidium (DHE) that was oxidized by each ROS, enabling tracking of the radiation dose emitted by the nanoradiator. In the range 70 µm below the irradiated cell, ^\\bullet{\\rm{OH}} radicals derived mostly from either incident X-ray or X-ray fluorescence of ION nanoradiators are distributed along the line of depth direction in ROS gel. In contrast, {\\rm{O}}_2^- derived from secondary electron or low-energy electron emission by ION nanoradiators are scattered over the ROS gel. ROS fluorescence due to the ION nanoradiators was observed continuously to a depth of 1.5 mm for both oxidized APF and oxidized DHE with relatively large intensity compared with the fluorescence caused by the ROS produced solely by incident primary X-rays, which was limited to a depth of 600 µm, suggesting dose enhancement as well as more penetration by nanoradiators. In conclusion, the combined use of a synchrotron X-ray microbeam-irradiated three-dimensional ROS gel and confocal laser scanning fluorescence microscopy provides a simple dosimetry method for track analysis of X-ray photoelectric nanoradiator radiation, suggesting extensive cellular damage with dose-enhancement beyond a single cell containing IONs.

  1. Trace-metal sources and their release from mine wastes: examples from humidity cell tests of hardrock mine waste and from Warrior Basin coal

    USGS Publications Warehouse

    Diehl, S.F.; Smith, Kathleen S.; Desborough, G.A.; White, W.W.; Lapakko, K.A.; Goldhaber, Martin B.; Fey, David L.

    2003-01-01

    To assess the potential impact of metal and acid contamination from mine-waste piles, it is important to identify the mineralogic source of trace metals and their mode of occurrence. Microscopic analysis of mine-waste samples from both hard-rock and coalmine waste samples demonstrate a microstructural control, as well as mineralogic control, on the source and release of trace metals into local water systems. The samples discussed herein show multiple periods of sulfide mineralization with varying concentrations of trace metals. In the first case study, two proprietary hard-rock mine-waste samples exposed to a series of humidity cell tests (which simulate intense chemical weathering conditions) generated acid and released trace metals. Some trace elements of interest were: arsenic (45-120 ppm), copper (60-320 ppm), and zinc (30-2,500 ppm). Untested and humidity cell-exposed samples were studied by X-ray diffraction, scanning electron microscope with energy dispersive X-ray (SEM/EDX), and electron microprobe analysis. Studies of one sample set revealed arsenic-bearing pyrite in early iron- and magnesium-rich carbonate-filled microveins, and iron-, copper-, arsenic-, antimony-bearing sulfides in later crosscutting silica-filled microveins. Post humidity cell tests indicated that the carbonate minerals were removed by leaching in the humidity cells, exposing pyrite to oxidative conditions. However, sulfides in the silica-filled veins were more protected. Therefore, the trace metals contained in the sulfides within the silica-filled microveins may be released to the surface and (or) ground water system more slowly over a greater time period. In the second case study, trace metal-rich pyrite-bearing coals from the Warrior Basin, Alabama were analyzed. Arsenic-bearing pyrite was observed in a late-stage pyrite phase in microfaults and microveins that crosscut earlier arsenic.

  2. Thermochronological evolution of an intra-plate magmatic event inferred from an integrated modeling approach: A case study in the Westerwald, Germany

    NASA Astrophysics Data System (ADS)

    Tirone, M.; Rokitta, K.; Schreiber, U.

    2016-09-01

    A lava sample from the Tertiary Westerwald volcanic field was selected for a detailed study using various analytical techniques in combination with petrological, thermodynamic and diffusion modeling to extract information related to the thermochronological evolution of a magmatic event before eruption. The lava sample contains large olivine phenocrysts which are compositionally zoned and two coexisting but chemically distinct melts, a host melt with basaltic composition and small spherical pockets of a less abundant trachytic melt (globules). The sample was analyzed by electron microprobe, x-ray fluorescence (XRF) X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). The primary melt of the host lava was determined using the program PRIMELT2.XLS. Partial fractional crystallization of olivine was modeled using the program alphaMELTS. Timescale and cooling rate were retrieved by fitting the measured Fe-Mg zoning along two directions in four olivine grains from the host lava using a 3-D numerical diffusion model. The measured variation of Ca is also consistent with a chemical diffusion process, while a numerical growth model applied to the same olivines does not appear to explain the Fe-Mg zoning. Chemical zoning of major elements in the melt globules were reproduced with a multicomponent diffusion model. The results of this study show that the host magma fractionated about 9% of olivine in a first stage, then the crystallization proceeded without further separation of mineral phases. Modeling of diffusion in the olivine crystals suggests that this second stage lasted at least 5 yrs and the temperature of the melt decreased from 1120-1150 °C to 1090 °C during this time. According to the results of the multicomponent diffusion model applied to the melt globules, the coexistence of the two melts was extremely short (less than few hours), possibly recording the assimilation of the globules during eruption or cooling of the whole system on the surface.

  3. Coordinated STEM/FIB/NanoSIMS Analyses of Presolar Silicates in Comet Dust and Primitive Meteorites

    NASA Technical Reports Server (NTRS)

    Keller, Lindsay; Nguyen, A.; Rahman, Z.; Messenger, S.

    2012-01-01

    Silicate grains were among the most abundant mineralogical building blocks of our Solar System. These grains were the detritus from earlier generations of stars that have been recycled in the early solar nebula. Rare sub-micrometer survivors of this processing have been identified in meteorites, micrometeorites and interplanetary dust particles (IDPs). These silicate grains are recognized as presolar in origin because of their extremely anomalous isotopic compositions that reflect nucleosynthetic processes in their stellar sources (evolved stars, novae and supernovae). We perform coordinated chemical, mineralogical and isotopic studies of these grains to determine their origins and histories. We examine the complex mineralogy and petrography of presolar silicates using imaging, diffraction and chemical data obtained from thin sections with the JSC JEOL 2500 field-emission STEM equipped with a Noran thin window energy dispersive x-ray (EDX) spectrometer and a Gatan Tridiem GIF. Quantitative element x-ray maps (spectrum images) are acquired by rastering a 4 nm incident probe whose dwell time is minimized to avoid beam damage and element diffusion during mapping. Successive image layers are acquired and combined in order to achieve approx 1% counting statistics for major elements. The IDP samples are prepared by ultramicrotomy of particles embedded in epoxy or elemental sulfur. After EDX mapping, the sections are subjected to C, N, and O isotopic imaging with the JSC NanoSIMS 50L ion microprobe. We prepare sections of some meteorite grains using the JSC FEI Quanta 3D focused ion beam (FIB) instrument. The specimen surface is protected from the FIB milling process by layers of electron beam-deposited C and Pt followed by an ion-deposited Pt layer. We also use the FIB to preferentially remove surrounding grains to reduce the background in subsequent NanoSIMS measurements. For mineralogical studies, we again employ the FIB instrument to deposit a protective cap over the grain of interest and then extract the grain and thin it to electron transparency for TEM analysis.

  4. X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser

    DOE PAGES

    Kroll, Thomas; Kern, Jan; Kubin, Markus; ...

    2016-09-19

    X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. But, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatization is needed. We compare L-edge x-ray absorption spectroscopy (XAS) of a prototypical transition metal system based on monochromatizing the SASE radiation of the linac coherent light source (LCLS) with a new technique based onmore » self-seeding of LCLS. We demonstrate how L-edge XAS can be performed using the self-seeding scheme without the need of an additional beam line monochromator. Lastly, we show how the spectral shape and pulse energy depend on the undulator setup and how this affects the x-ray spectroscopy measurements.« less

  5. X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser

    PubMed Central

    Kroll, Thomas; Kern, Jan; Kubin, Markus; Ratner, Daniel; Gul, Sheraz; Fuller, Franklin D.; Löchel, Heike; Krzywinski, Jacek; Lutman, Alberto; Ding, Yuantao; Dakovski, Georgi L.; Moeller, Stefan; Turner, Joshua J.; Alonso-Mori, Roberto; Nordlund, Dennis L.; Rehanek, Jens; Weniger, Christian; Firsov, Alexander; Brzhezinskaya, Maria; Chatterjee, Ruchira; Lassalle-Kaiser, Benedikt; Sierra, Raymond G.; Laksmono, Hartawan; Hill, Ethan; Borovik, Andrew; Erko, Alexei; Föhlisch, Alexander; Mitzner, Rolf; Yachandra, Vittal K.; Yano, Junko; Wernet, Philippe; Bergmann, Uwe

    2016-01-01

    X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. However, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatization is needed. Here we compare L-edge x-ray absorption spectroscopy (XAS) of a prototypical transition metal system based on monochromatizing the SASE radiation of the linac coherent light source (LCLS) with a new technique based on self-seeding of LCLS. We demonstrate how L-edge XAS can be performed using the self-seeding scheme without the need of an additional beam line monochromator. We show how the spectral shape and pulse energy depend on the undulator setup and how this affects the x-ray spectroscopy measurements. PMID:27828320

  6. IBIC characterisation of novel detectors for single atom doping of quantum computer devices

    NASA Astrophysics Data System (ADS)

    Yang, Changyi; Jamieson, David N.; Pakes, Chris I.; George, Damien P.; Hearne, Sean M.; Dzurak, Andrew S.; Gauja, Eric; Stanley, F.; Clark, R. G.

    2003-09-01

    Single ion implantation and online detection is highly desirable for the emerging application, in which single 31P ions need to be inserted in prefabricated silicon cells to construct solid-state quantum bits (qubits). In order to fabricate qubit arrays, we have developed novel detectors that employ detector electrodes adjacent to the prefabricated cells that can detect single keV ion strikes appropriate for the fabrication of shallow phosphorus arrays. The method utilises a high purity silicon substrate with very high resistivity, a thin SiO 2 surface layer, nanometer masks for the lateral positioning single phosphorus implantation, biased electrodes applied to the surface of the silicon and sensitive electronics that can detect the charge transient from single keV ion strikes. A TCAD (Technology Computer Aided Design) software package was applied in the optimisation of the device design and simulation of the detector performance. Here we show the characterisation of these detectors using ion beam induced charge (IBIC) with a focused 2 MeV He ions in a nuclear microprobe. The IBIC imaging method in a nuclear microprobe allowed us to measure the dead-layer thickness of the detector structure (required to be very thin for successful detection of keV ions), and the spatial distribution of the charge collection efficiency around the entire region of the detector. We show that our detectors have near 100% charge collection efficiency for MeV ions, extremely thin dead-layer thickness (about 7 nm) and a wide active region extending laterally from the electrodes (10-20 μm) where qubit arrays can be constructed. We demonstrate that the device can be successfully applied in the detection of keV ionisation energy from single events of keV X-rays and keV 31P ions.

  7. The structure of denisovite, a fibrous nanocrystalline polytypic disordered ‘very complex’ silicate, studied by a synergistic multi-disciplinary approach employing methods of electron crystallography and X-ray powder diffraction

    PubMed Central

    Schowalter, Marco; Schmidt, Martin U.; Czank, Michael; Depmeier, Wulf; Rosenauer, Andreas

    2017-01-01

    Denisovite is a rare mineral occurring as aggregates of fibres typically 200–500 nm diameter. It was confirmed as a new mineral in 1984, but important facts about its chemical formula, lattice parameters, symmetry and structure have remained incompletely known since then. Recently obtained results from studies using microprobe analysis, X-ray powder diffraction (XRPD), electron crystallography, modelling and Rietveld refinement will be reported. The electron crystallography methods include transmission electron microscopy (TEM), selected-area electron diffraction (SAED), high-angle annular dark-field imaging (HAADF), high-resolution transmission electron microscopy (HRTEM), precession electron diffraction (PED) and electron diffraction tomography (EDT). A structural model of denisovite was developed from HAADF images and later completed on the basis of quasi-kinematic EDT data by ab initio structure solution using direct methods and least-squares refinement. The model was confirmed by Rietveld refinement. The lattice parameters are a = 31.024 (1), b = 19.554 (1) and c = 7.1441 (5) Å, β = 95.99 (3)°, V = 4310.1 (5) Å3 and space group P12/a1. The structure consists of three topologically distinct dreier silicate chains, viz. two xonotlite-like dreier double chains, [Si6O17]10−, and a tubular loop-branched dreier triple chain, [Si12O30]12−. The silicate chains occur between three walls of edge-sharing (Ca,Na) octahedra. The chains of silicate tetrahedra and the octahedra walls extend parallel to the z axis and form a layer parallel to (100). Water molecules and K+ cations are located at the centre of the tubular silicate chain. The latter also occupy positions close to the centres of eight-membered rings in the silicate chains. The silicate chains are geometrically constrained by neighbouring octahedra walls and present an ambiguity with respect to their z position along these walls, with displacements between neighbouring layers being either Δz = c/4 or −c/4. Such behaviour is typical for polytypic sequences and leads to disorder along [100]. In fact, the diffraction pattern does not show any sharp reflections with l odd, but continuous diffuse streaks parallel to a* instead. Only reflections with l even are sharp. The diffuse scattering is caused by (100) nano­lamellae separated by stacking faults and twin boundaries. The structure can be described according to the order–disorder (OD) theory as a stacking of layers parallel to (100). PMID:28512570

  8. Trace element analysis by EPMA in geosciences: detection limit, precision and accuracy

    NASA Astrophysics Data System (ADS)

    Batanova, V. G.; Sobolev, A. V.; Magnin, V.

    2018-01-01

    Use of the electron probe microanalyser (EPMA) for trace element analysis has increased over the last decade, mainly because of improved stability of spectrometers and the electron column when operated at high probe current; development of new large-area crystal monochromators and ultra-high count rate spectrometers; full integration of energy-dispersive / wavelength-dispersive X-ray spectrometry (EDS/WDS) signals; and the development of powerful software packages. For phases that are stable under a dense electron beam, the detection limit and precision can be decreased to the ppm level by using high acceleration voltage and beam current combined with long counting time. Data on 10 elements (Na, Al, P, Ca, Ti, Cr, Mn, Co, Ni, Zn) in olivine obtained on a JEOL JXA-8230 microprobe with tungsten filament show that the detection limit decreases proportionally to the square root of counting time and probe current. For all elements equal or heavier than phosphorus (Z = 15), the detection limit decreases with increasing accelerating voltage. The analytical precision for minor and trace elements analysed in olivine at 25 kV accelerating voltage and 900 nA beam current is 4 - 18 ppm (2 standard deviations of repeated measurements of the olivine reference sample) and is similar to the detection limit of corresponding elements. To analyse trace elements accurately requires careful estimation of background, and consideration of sample damage under the beam and secondary fluorescence from phase boundaries. The development and use of matrix reference samples with well-characterised trace elements of interest is important for monitoring and improving of the accuracy. An evaluation of the accuracy of trace element analyses in olivine has been made by comparing EPMA data for new reference samples with data obtained by different in-situ and bulk analytical methods in six different laboratories worldwide. For all elements, the measured concentrations in the olivine reference sample were found to be identical (within internal precision) to reference values, suggesting that achieved precision and accuracy are similar. The spatial resolution of EPMA in a silicate matrix, even at very extreme conditions (accelerating voltage 25 kV), does not exceed 7 - 8 μm and thus is still better than laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) or secondary ion mass spectrometry (SIMS) of similar precision. These make the electron microprobe an indispensable method with applications in experimental petrology, geochemistry and cosmochemistry.

  9. Electron acceleration in pulsed-power driven magnetic-reconnection experiments

    NASA Astrophysics Data System (ADS)

    Halliday, Jonathan; Hare, Jack; Lebedev, Sergey; Suttle, Lee; Bland, Simon; Clayson, Thomas; Tubman, Eleanor; Pikuz, Sergei; Shelkovenko, Tanya

    2017-10-01

    We present recent results from pulsed-power driven magnetic reconnection experiments, fielded on the MAGPIE generator (1.2 MA, 250 ns). The setup used in these experiments produces plasma inflows which are intrinsically magnetised; persist for many hydrodynamic time-scales; and are supersonic. Previous work has focussed on characterising the dynamics of bulk plasma flows, using a suite of diagnostics including laser interferometry, (imaging) Faraday rotation, and Thompson scattering. Measurements show the formation of a well defined, long lasting reconnection layer and demonstrate a power balance between the power into and out of the reconnection region. The work presented here focuses on diagnosing non-thermal electron acceleration by the reconnecting electric field. To achieve this, metal foils were placed in the path of accelerated electrons. Atomic transitions in the foil were collisionally exited by the electron beam, producing a characteristic X-Ray spectrum. This X-Ray emission was diagnosed using spherically bent crystal X-Ray spectrometry, filtered X-Ray pinhole imaging, and X-Ray sensitive PIN diodes.

  10. Prediction and Measurement of X-Ray Spectral and Intensity Distributions from Low Energy Electron Impact Sources

    NASA Technical Reports Server (NTRS)

    Edwards, David L.

    1999-01-01

    In-vacuum electron beam welding is a technology that NASA considered as a joining technique for manufacture of space structures. The interaction of energetic electrons with metal produces x-rays. The radiation exposure to astronauts performing the in-vacuum electron beam welding must be characterized and minimized to insure safe operating conditions. This investigation characterized the x-ray environment due to operation of an in-vacuum electron beam welding tool. NASA, in a joint venture with the Russian Space Agency, was scheduled to perform a series of welding in space experiments on board the United States Space Shuttle. This series of experiments was named the International Space Welding Experiment (ISWE). The hardware associated with the ISWE was leased to NASA, by the Paton Welding Institute (PWI) in Ukraine, for ground based welding experiments in preparation for flight. Two tests were scheduled, using the ISWE electron beam welding tool, to characterize the radiation exposure to an astronaut during the operation of the ISWE. These radiation exposure tests consisted of Thermoluminescence Dosimeters (TLD's) shielded with material currently used by astronauts during Extra Vehicular Activities (EVA) and exposed to x-ray radiation generated by operation of an in-vacuum electron beam welding tool. This investigation was the first known application of TLD's to measure absorbed dose from x-rays of energy less than 10 KeV. The ISWE hardware was returned to Ukraine before the issue of adequate shielding for the astronauts was verified. Therefore, alternate experimental and analytical methods were developed to measure and predict the x-ray spectral and intensity distribution generated by electron impact with metal. These x-ray spectra were used to calculate the absorbed radiation dose to astronauts. These absorbed dose values were compared to TLD measurements obtained during actual operation of the in-vacuum electron beam welding tool. The calculated absorbed dose values were found to be in good agreement with the TLD values.

  11. High-Performance X-ray Detection in a New Analytical Electron Microscope

    NASA Technical Reports Server (NTRS)

    Lyman, C. E.; Goldstein, J. I.; Williams, D. B.; Ackland, D. W.; vonHarrach, S.; Nicholls, A. W.; Statham, P. J.

    1994-01-01

    X-ray detection by energy-dispersive spectrometry in the analytical electron microscope (AEM) is often limited by low collected X-ray intensity (P), modest peak-to-background (P/B) ratios, and limitations on total counting time (tau) due to specimen drift and contamination. A new AFM has been designed with maximization of P. P/B, and tau as the primary considerations. Maximization of P has been accomplished by employing a field-emission electron gun, X-ray detectors with high collection angles, high-speed beam blanking to allow only one photon into the detector at a time, and simultaneous collection from two detectors. P/B has been maximized by reducing extraneous background signals generated at the specimen holder, the polepieces and the detector collimator. The maximum practical tau has been increased by reducing specimen contamination and employing electronic drift correction. Performance improvments have been measured using the NIST standard Cr thin film. The 0-3 steradian solid angle of X-ray collection is the highest value available. The beam blanking scheme for X-ray detection provides 3-4 times greater throughput of X-rays at high count rates into a recorded spectrum than normal systems employing pulse-pileup rejection circuits. Simultaneous X-ray collection from two detectors allows the highest X-ray intensity yet recorded to be collected from the NIST Cr thin film. The measured P/B of 6300 is the highest level recorded for an AEM. In addition to collected X-ray intensity (cps/nA) and P/B measured on the standard Cr film, the product of these can be used as a figure-of-merit to evaluate instruments. Estimated minimum mass fraction (MMF) for Cr measured on the standard NIST Cr thin film is also proposed as a figure-of-merit for comparing X-ray detection in AEMs. Determinations here of the MMF of Cr detectable show at least a threefold improvement over previous instruments.

  12. A Many-Body Formalism of ΔSCF Approach for Simulating X-Ray Spectra from First-Principles

    NASA Astrophysics Data System (ADS)

    Liang, Yufeng; Vinson, John; Pemmaraju, Sri; Drisdell, Walter; Shirley, Eric; Prendegast, David

    Accurately reproducing X-ray spectral fingerprints for materials characterization relies heavily on how to correctly model the many-electron response to the generation of an X-ray core hole. In this talk, we present a novel first-principles theory for simulating X-ray spectra that is based on many-electron wavefunctions. The proposed theory go beyond the electron-hole correlations within the Bethe-Saltpeter Equation and consider higher-order vertex corrections up to the level of Mahan-Noziéres-De Dominicis (MND) theory. An efficient algorithm is invented to incorporate these many-electron processes by using linear algebra rather than iterating over all Feynman diag United States Department of Energy under Contact No. DE-AC02-05CH11231, No. DE-SC0004993.

  13. Observation of Betatron X-Ray Radiation in a Self-Modulated Laser Wakefield Accelerator Driven with Picosecond Laser Pulses

    DOE PAGES

    Albert, F.; Lemos, N.; Shaw, J. L.; ...

    2017-03-31

    We investigate a new regime for betatron x-ray emission that utilizes kilojoule-class picosecond lasers to drive wakes in plasmas. When such laser pulses with intensities of ~ 5 × 1 0 18 W / cm 2 are focused into plasmas with electron densities of ~ 1 × 1 0 19 cm - 3 , they undergo self-modulation and channeling, which accelerates electrons up to 200 MeV energies and causes those electrons to emit x rays. The measured x-ray spectra are fit with a synchrotron spectrum with a critical energy of 10–20 keV, and 2D particle-in-cell simulations were used to modelmore » the acceleration and radiation of the electrons in our experimental conditions« less

  14. Overview of options for generating high-brightness attosecond x-ray pulses at free-electron lasers and applications at the European XFEL

    NASA Astrophysics Data System (ADS)

    Serkez, S.; Geloni, G.; Tomin, S.; Feng, G.; Gryzlova, E. V.; Grum-Grzhimailo, A. N.; Meyer, M.

    2018-02-01

    The generation of attosecond, highbrightness x-ray pulses is a matter of great interest given their applications in the study of ultra-fast processes. In recent years, the production of x-ray pulses of high brightness, both in the soft and in the hard x-ray range, has been enabled by x-ray free-electron lasers (XFELs). In contrast to conventional quantum lasers, XFELs are based on the use of an ultra-relativistic electron beam as gain medium. They often work in the self-amplified spontaneous emission (SASE) regime, which provides pulses of duration down to a few femtoseconds, composed of several longitudinal modes. In order to further decrease the duration of these pulses, special methods need to be implemented. In this paper we review available methods, with particular focus on the x-ray laser-enhanced attosecond pulse generation, which is one of the most promising techniques. We illustrate the method using the SASE3 soft x-ray undulator of the European XFEL facility as a case study, emphasizing the importance of high-repetition rate attosecond x-ray pulses. The expected attosecond-level radiation output is used for simulations of sequential ionization processes in atoms in the case of ionization in the soft x-ray regime, demonstrating the importance of this opportunity for the user community.

  15. Soft x-ray spectroscopy studies of novel electronic materials using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Newby, David, Jr.

    Soft x-ray spectroscopy can provide a wealth of information on the electronic structure of solids. In this work, a suite of soft x-ray spectroscopies is applied to organic and inorganic materials with potential applications in electronic and energy generation devices. Using the techniques of x-ray absorption (XAS), x-ray emission spectroscopy (XES), and x-ray photoemission spectroscopy (XPS), the fundamental properties of these different materials are explored. Cycloparaphenylenes (CPPs) are a recently synthesized family of cyclic hydrocarbons with very interesting properties and many potential applications. Unusual UV/Visible fluorescence trends have spurred a number of theoretical investigations into the electronic properties of the CPP family, but thus far no comprehensive electronic structure measurements have been conducted. XPS, XAS, and XES data for two varieties, [8]- and [10]-CPP, are presented here, and compared with the results of relevant DFT calculations. Turning towards more application-centered investigations, similar measurements are applied to two materials commonly used in solid oxide fuel cell (SOFC) cathodes: La1-xSrxMnO 3 (LSMO) and La1-xSr1- xCo1-yFe yO3 (LSCF). Both materials are structurally perovskites, but they exhibit strikingly different electronic properties. SOFC systems very efficiently produce electricity by catalyzing reactions between oxygen and petroleum-based hydrocarbons at high temperatures (> 800 C). Such systems are already utilized to great effect in many industries, but more widespread adoption could be had if the cells could operate at lower temperatures. Understanding the electronic structure and operational evolution of the cathode materials is essential for the development of better low-temperature fuel cells. LSCF is a mixed ion-electron conductor which holds promise for low-temperature SOFC applications. XPS spectra of LSCF thin films are collected as the films are heated and gas-dosed in a controlled environment. The surface evolution of these films is discussed, and the effects of different gas environments on oxygen vacancy concentration are elucidated. LSMO is commonly used in commercial fuel cell devices. Here the resonant soft x-ray emission (RIXS) spectrum of LSMO is examined, and it is shown that the inelastic x-ray emission structure of LSMO arises from local atomic multiplet effects.

  16. Nanoplasma Formation by High Intensity Hard X-rays

    PubMed Central

    Tachibana, T.; Jurek, Z.; Fukuzawa, H.; Motomura, K.; Nagaya, K.; Wada, S.; Johnsson, P.; Siano, M.; Mondal, S.; Ito, Y.; Kimura, M.; Sakai, T.; Matsunami, K.; Hayashita, H.; Kajikawa, J.; Liu, X.-J.; Robert, E.; Miron, C.; Feifel, R.; Marangos, J. P.; Tono, K.; Inubushi, Y.; Yabashi, M.; Son, S.-K.; Ziaja, B.; Yao, M.; Santra, R.; Ueda, K.

    2015-01-01

    Using electron spectroscopy, we have investigated nanoplasma formation from noble gas clusters exposed to high-intensity hard-x-ray pulses at ~5 keV. Our experiment was carried out at the SPring-8 Angstrom Compact free electron LAser (SACLA) facility in Japan. Dedicated theoretical simulations were performed with the molecular dynamics tool XMDYN. We found that in this unprecedented wavelength regime nanoplasma formation is a highly indirect process. In the argon clusters investigated, nanoplasma is mainly formed through secondary electron cascading initiated by slow Auger electrons. Energy is distributed within the sample entirely through Auger processes and secondary electron cascading following photoabsorption, as in the hard x-ray regime there is no direct energy transfer from the field to the plasma. This plasma formation mechanism is specific to the hard-x-ray regime and may, thus, also be important for XFEL-based molecular imaging studies. In xenon clusters, photo- and Auger electrons contribute more significantly to the nanoplasma formation. Good agreement between experiment and simulations validates our modelling approach. This has wide-ranging implications for our ability to quantitatively predict the behavior of complex molecular systems irradiated by high-intensity hard x-rays. PMID:26077863

  17. Lightning leader models of terrestrial gamma-ray flashes

    NASA Astrophysics Data System (ADS)

    Dwyer, J. R.; Liu, N.; Ihaddadene, K. M. A.

    2017-12-01

    Terrestrial gamma-ray flashes (TGFs) are bright sub-millisecond bursts of gamma rays that originate from thunderstorms. Because lightning leaders near the ground have been observed to emit x-rays, presumably due to runaway electron production in the high-field regions near the leader tips, models of TGFs have been developed by several groups that assume a similar production mechanism of runaway electrons from lightning leaders propagating through thunderclouds. However, it remains unclear exactly how and where these runaway electrons are produced, since lightning propagation at thunderstorm altitudes remains poorly understood. In addition, it is not obvious how to connect the observed behavior of the x-ray production from lightning near the ground with the properties of TGFs. For example, it is not clear how to relate the time structure of the x-ray emission near the ground to that of TGFs, since x-rays from stepped leaders near the ground are usually produced in a series of sub-microsecond bursts, but TGFs are usually observed as much longer pulses without clear substructures, at sub-microsecond timescales or otherwise. In this presentation, spacecraft observations of TGFs, ground-based observations of x-rays from lightning and laboratory sparks, and Monte Carlo and PIC simulations of runaway electron and gamma ray production and propagation will be used to constrain the lightning leader models of TGFs.

  18. Geological applications of synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Henderson, C. M. B.; Cressey, G.; Redfern, S. A. T.

    1995-03-01

    Synchrotron-based, Earth sciences research carried out over the last 5 years is reviewed with special attention being given to X-ray absorption studies; X-ray diffraction and X-ray fluorescence microprobe applications are considered more briefly. A comprehensive bibliography is included. The main part of the paper summarizes recent work carried out at the Daresbury SRS. K-edge XAS studies of glasses as models for silicate melts provide information on the local structural environments of Si, Fe 2+ and Fe 3+. By analogy with synthetic "leucites" which contain Fe 2+ and Fe 3+ in tetrahedral framework sites, it seems that many model glasses also contain both oxidation states of Fe in the network, rather than as network modifiers. The structural sites occupied by the minor elements Mn, Zn and Ti in staurolite have been identified using XAFS; Mn and Zn substitute for Fe 2+ in the tetrahedral T2 site, while Ti occupies the distorted M2 octahedral site. L-edge spectroscopy is used to identify the valencies and electronic structures of Mn and Fe in minerals and the Fe 2+:Fe 3+ ratio in a natural spinel is determined. The polarized nature of the synchrotron beam is exploited in determining the Fe X-ray absorption anisotropy in single crystal tourmaline and epidote. XRD powder studies include Rietveld-refinement structure determination and compressibility studies. Synthetic "leucites" having the stoichiometry K 2MgSi 5O 12 have distinctly different structures. The dry-synthesized form is cubic Ia3d with Si and Mg fully disordered on tetrahedral framework sites, while the hydrothermally-synthesized polymorph is monoclinic P2 1/c with Si and Mg fully disordered on, respectively, 10 and 2 tetrahedral sites. The reversible tetragonal to orthorhombic phase transition in gillespite (BaFeSi 4O 10) has been studied in a diamond anvil cell using ED detection and found to occur at 1.2 ± 0.1 GPa. The anomalous compressibility observed has been interpreted in terms of ferroelastic and coelastic phenomena and the related order parameters analysed using Landau theory. The compressibility of MgCO 3, determined up to 20 GPa, has been combined with thermochemical data to obtain an "equation to state" for magnesite and it is found that magnesite is likely to be the main host for carbon in the Earth's lower mantle.

  19. Unusual Kondo-hole effect and crystal-field frustration in Nd-doped CeRhIn 5

    DOE PAGES

    Rosa, Priscila Ferrari Silveira; Oostra, Aaron; Thompson, Joe David; ...

    2016-07-05

    In this research, we investigate single crystals of Ce 1₋xNd xRhIn 5 by means of x-ray-diffraction, microprobe, magnetic susceptibility, heat capacity, and electrical resistivity measurements. Our data reveal that the antiferromagnetic transition of CeRhIn 5, at Tmore » $$Ce\\atop{N}$$=3.8 K, is linearly suppressed with x Nd. We associate this effect with the presence of a “Kondo hole” created by Nd substitution. The extrapolation of T$$Ce\\atop{N}$$ to zero temperature, however, occurs at x c~0.3, which is below the two-dimensional percolation limit found in Ce 1₋xLa xRhIn 5. This result strongly suggests the presence of a crystal-field induced magnetic frustration. Near x Nd~0.2, the Ising antiferromagnetic order from Nd 3+ ions is stabilized and T$$Nd\\atop{N}$$ increases up to 11 K in NdRhIn 5. Finally, our results shed light on the effects of magnetic doping in heavy-fermion antiferromagnets and stimulate the study of such systems under applied pressure.« less

  20. Electronic Structure of the Organic Semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from Soft X-ray Spectroscopies and Density Functional Theory Calculations

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

    DeMasi, A.; Piper, L; Zhang, Y

    2008-01-01

    The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq3) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq3, and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studiesmore » and the present data reveal the presence of clear photon-induced damage in the former.« less

  1. First refraction contrast imaging via Laser-Compton Scattering X-ray at KEK

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

    Sakaue, Kazuyuki; Aoki, Tatsuro; Washio, Masakazu

    2012-07-31

    Laser-Compton Scattering (LCS) is one of the most feasible techniques for high quality, high brightness, and compact X-ray source. High energy electron beam produced by accelerators scatters off the laser photon at a small spot. As a laser target, we have been developing a pulsedlaser storage cavity for increasing an X-ray flux. The X-ray flux was still inadequate that was 2.1 Multiplication-Sign 10{sup 5}/sec, however, we performed first refraction contrast imaging in order to evaluate the quality of LCS X-ray. Edge enhanced contrast imaging was achieved by changing the distance from sample to detector. The edge enhancement indicates that themore » LCS X-ray has small source size, i.e. high brightness. We believe that the result has demonstrated good feasibility of linac-based high brightness X-ray sources via laser-electron Compton scatterings.« less

  2. 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

  3. Electron cyclotron resonance ion source plasma characterization by X-ray spectroscopy and X-ray imaging

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

    Mascali, David, E-mail: davidmascali@lns.infn.it; Castro, Giuseppe; Celona, Luigi

    2016-02-15

    An experimental campaign aiming to investigate electron cyclotron resonance (ECR) plasma X-ray emission has been recently carried out at the ECRISs—Electron Cyclotron Resonance Ion Sources laboratory of Atomki based on a collaboration between the Debrecen and Catania ECR teams. In a first series, the X-ray spectroscopy was performed through silicon drift detectors and high purity germanium detectors, characterizing the volumetric plasma emission. The on-purpose developed collimation system was suitable for direct plasma density evaluation, performed “on-line” during beam extraction and charge state distribution characterization. A campaign for correlating the plasma density and temperature with the output charge states and themore » beam intensity for different pumping wave frequencies, different magnetic field profiles, and single-gas/gas-mixing configurations was carried out. The results reveal a surprisingly very good agreement between warm-electron density fluctuations, output beam currents, and the calculated electromagnetic modal density of the plasma chamber. A charge-coupled device camera coupled to a small pin-hole allowing X-ray imaging was installed and numerous X-ray photos were taken in order to study the peculiarities of the ECRIS plasma structure.« less

  4. Decimetric type III radio bursts and associated hard X-ray spikes

    NASA Technical Reports Server (NTRS)

    Dennis, B. R.; Benz, A. O.; Ranieri, M.; Simnett, G. M.

    1984-01-01

    For a relatively weak solar flare on August 6, 1981, at 10:32 UT, a detailed comparison is made between hard X-ray spikes and decimetric type III radio bursts. The hard X-ray observations are made at energies above 30 keV, and the radio data are obtained in the frequency range from 100 to 1000 MHz. The time resolution for all the data sets is approximately 0.1 s or better. The dynamic radio spectrum exhibits many fast drift type III radio bursts with both normal and reverse slope, whereas the X-ray time profile contains many well resolved short spikes with durations less than or equal to 1 s. Some of the X-ray spikes are seen to be associated in time with reverse-slope bursts, indicating either that the electron beams producing the radio burst contain two or three orders of magnitude more fast electrons than has previously been assumed or that the electron beams can induce the acceleration of additional electrons or occur in coincidence with this acceleration. A case is presented in which a normal slope radio burst at approximately 600 MHz occurs in coincidence with the peak of an X-ray spike to within 0.1 s.

  5. X-ray Observations of Cosmic Ray Acceleration

    NASA Technical Reports Server (NTRS)

    Petre, Robert

    2012-01-01

    Since the discovery of cosmic rays, detection of their sources has remained elusive. A major breakthrough has come through the identification of synchrotron X-rays from the shocks of supernova remnants through imaging and spectroscopic observations by the most recent generation of X-ray observatories. This radiation is most likely produced by electrons accelerated to relativistic energy, and thus has offered the first, albeit indirect, observational evidence that diffusive shock acceleration in supernova remnants produces cosmic rays to TeV energies, possibly as high as the "knee" in the cosmic ray spectrum. X-ray observations have provided information about the maximum energy to which these shOCks accelerate electrons, as well as indirect evidence of proton acceleration. Shock morphologies measured in X-rays have indicated that a substantial fraction of the shock energy can be diverted into particle acceleration. This presentation will summarize what we have learned about cosmic ray acceleration from X-ray observations of supernova remnants over the past two decades.

  6. Talbot-Lau x-ray deflectometer electron density diagnostic for laser and pulsed power high energy density plasma experiments (invited).

    PubMed

    Valdivia, M P; Stutman, D; Stoeckl, C; Mileham, C; Begishev, I A; Theobald, W; Bromage, J; Regan, S P; Klein, S R; Muñoz-Cordovez, G; Vescovi, M; Valenzuela-Villaseca, V; Veloso, F

    2016-11-01

    Talbot-Lau X-ray deflectometry (TXD) has been developed as an electron density diagnostic for High Energy Density (HED) plasmas. The technique can deliver x-ray refraction, attenuation, elemental composition, and scatter information from a single Moiré image. An 8 keV Talbot-Lau interferometer was deployed using laser and x-pinch backlighters. Grating survival and electron density mapping were demonstrated for 25-29 J, 8-30 ps laser pulses using copper foil targets. Moiré pattern formation and grating survival were also observed using a copper x-pinch driven at 400 kA, ∼1 kA/ns. These results demonstrate the potential of TXD as an electron density diagnostic for HED plasmas.

  7. Talbot-Lau X-ray Deflectometer electron density diagnostic for laser and pulsed power high energy density plasma experiments

    DOE PAGES

    Valdivia, M. P.; Stutman, D.; Stoeckl, C.; ...

    2016-04-21

    Talbot-Lau X-ray Deflectometry has been developed as an electron density diagnostic for High Energy Density plasmas. The technique can deliver x-ray refraction, attenuation, elemental composition, and scatter information from a single Moiré image. An 8 keV Talbot-Lau interferometer was deployed using laser and x-pinch backlighters. Grating survival and electron density mapping was demonstrated for 25-29 J, 8-30 ps laser pulses using copper foil targets. Moire pattern formation and grating survival was also observed using a copper x-pinch driven at 400 kA, ~1 kA/ns. Lastly, these results demonstrate the potential of TXD as an electron density diagnostic for HED plasmas.

  8. 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.

  9. THz pulse doubler at FLASH: double pulses for pump–probe experiments at X-ray FELs

    PubMed Central

    Zapolnova, Ekaterina; Golz, Torsten; Pan, Rui; Klose, Karsten; Stojanovic, Nikola

    2018-01-01

    FLASH, the X-ray free-electron laser in Hamburg, Germany, employs a narrowband high-field accelerator THz source for unique THz pump X-ray probe experiments. However, the large difference in optical paths of the THz and X-ray beamlines prevents utilization of the machine’s full potential (e.g. extreme pulse energies in the soft X-ray range). To solve this issue, lasing of double electron bunches, separated by 28 periods of the driving radiofrequency (at 1.3 GHz), timed for the temporal overlap of THz and X-ray pulses at the experimental station has been employed. In order to optimize conditions for a typical THz pump X-ray probe experiment, X-ray lasing of the first bunch to one-sixth of that of the second has been suppressed. Finally, synchronization of THz radiation pulses was measured to be ∼20 fs (r.m.s.), and a solution for monitoring the arrival time for achieving higher temporal resolution is presented. PMID:29271749

  10. Selenium single-wavelength anomalous diffraction de novo phasing using an X-ray-free electron laser

    DOE PAGES

    Hunter, Mark S.; Yoon, Chun Hong; DeMirci, Hasan; ...

    2016-11-04

    Structural information about biological macromolecules near the atomic scale provides important insight into the functions of these molecules. To date, X-ray crystallography has been the predominant method used for macromolecular structure determination. However, challenges exist when solving structures with X-rays, including the phase problem and radiation damage. X-ray-free electron lasers (X-ray FELs) have enabled collection of diffraction information before the onset of radiation damage, yet the majority of structures solved at X-ray FELs have been phased using external information via molecular replacement. De novo phasing at X-ray FELs has proven challenging due in part to per-pulse variations in intensity andmore » wavelength. Here we report the solution of a selenobiotinyl-streptavidin structure using phases obtained by the anomalous diffraction of selenium measured at a single wavelength (Se-SAD) at the Linac Coherent Light Source. Finally, our results demonstrate Se-SAD, routinely employed at synchrotrons for novel structure determination, is now possible at X-ray FELs.« less

  11. THz pulse doubler at FLASH: double pulses for pump-probe experiments at X-ray FELs.

    PubMed

    Zapolnova, Ekaterina; Golz, Torsten; Pan, Rui; Klose, Karsten; Schreiber, Siegfried; Stojanovic, Nikola

    2018-01-01

    FLASH, the X-ray free-electron laser in Hamburg, Germany, employs a narrowband high-field accelerator THz source for unique THz pump X-ray probe experiments. However, the large difference in optical paths of the THz and X-ray beamlines prevents utilization of the machine's full potential (e.g. extreme pulse energies in the soft X-ray range). To solve this issue, lasing of double electron bunches, separated by 28 periods of the driving radiofrequency (at 1.3 GHz), timed for the temporal overlap of THz and X-ray pulses at the experimental station has been employed. In order to optimize conditions for a typical THz pump X-ray probe experiment, X-ray lasing of the first bunch to one-sixth of that of the second has been suppressed. Finally, synchronization of THz radiation pulses was measured to be ∼20 fs (r.m.s.), and a solution for monitoring the arrival time for achieving higher temporal resolution is presented.

  12. Geminga's tails: a pulsar bow shock probing the interstellar medium.

    PubMed

    Caraveo, P A; Bignami, G F; DeLuca, A; Mereghetti, S; Pellizzoni, A; Mignani, R; Tur, A; Becker, W

    2003-09-05

    We report the X-ray Multimirror Mission-Newton European Photon Imaging Camera observation of two elongated parallel x-ray tails trailing the pulsar Geminga. They are aligned with the object's supersonic motion, extend for approximately 2', and have a nonthermal spectrum produced by electron-synchrotron emission in the bow shock between the pulsar wind and the surrounding medium. Electron lifetime against synchrotron cooling matches the source transit time over the x-ray features' length. Such an x-ray detection of a pulsar bow shock (with no Halpha emission) allows us to gauge the pulsar electron injection energy and the shock magnetic field while constraining the angle of Geminga's motion and the local matter density.

  13. Ab initio calculation of the ion feature in x-ray Thomson scattering.

    PubMed

    Plagemann, Kai-Uwe; Rüter, Hannes R; Bornath, Thomas; Shihab, Mohammed; Desjarlais, Michael P; Fortmann, Carsten; Glenzer, Siegfried H; Redmer, Ronald

    2015-07-01

    The spectrum of x-ray Thomson scattering is proportional to the dynamic structure factor. An important contribution is the ion feature which describes elastic scattering of x rays off electrons. We apply an ab initio method for the calculation of the form factor of bound electrons, the slope of the screening cloud of free electrons, and the ion-ion structure factor in warm dense beryllium. With the presented method we can calculate the ion feature from first principles. These results will facilitate a better understanding of x-ray scattering in warm dense matter and an accurate measurement of ion temperatures which would allow determining nonequilibrium conditions, e.g., along shock propagation.

  14. X-ray magnetic circular dichroism and hard X-ray photoelectron spectroscopy of tetragonal Mn72Ge28 epitaxial thin film

    NASA Astrophysics Data System (ADS)

    Kim, Jinhyeok; Mizuguchi, Masaki; Inami, Nobuhito; Ueno, Tetsuro; Ueda, Shigenori; Takanashi, Koki

    2018-04-01

    An epitaxially grown Mn72Ge28 film with a tetragonal crystal structure was fabricated. It was clarified that the film had a perpendicular magnetization and a high perpendicular magnetic anisotropy energy of 14.3 Merg/cm3. The electronic structure was investigated by X-ray magnetic circular dichroism and hard X-ray photoelectron spectroscopy. The obtained X-ray magnetic circular dichroism spectrum revealed that the Mn orbital magnetic moment governed the magnetocrystalline anisotropy of the Mn72Ge28 film. A doublet structure was observed for the Mn 2p3/2 peak of hard X-ray photoelectron spectrum, indicating the spin exchange interaction between the 2p core-hole and 3d valence electrons.

  15. Laser x-ray Conversion and Electron Thermal Conductivity

    NASA Astrophysics Data System (ADS)

    Wang, Guang-yu; Chang, Tie-qiang

    2001-02-01

    The influence of electron thermal conductivity on the laser x-ray conversion in the coupling of 3ωo laser with Au plane target has been investigated by using a non-LTE radiation hydrodynamic code. The non-local electron thermal conductivity is introduced and compared with the other two kinds of the flux-limited Spitzer-Härm description. The results show that the non-local thermal conductivity causes the increase of the laser x-ray conversion efficiency and important changes of the plasma state and coupling feature.

  16. Specimen Holder for Analytical Electron Microscopes

    NASA Technical Reports Server (NTRS)

    Clanton, U. S.; Isaacs, A. M.; Mackinnon, I.

    1985-01-01

    Reduces spectral contamination by spurious X-ray. Specimen holder made of compressed carbon, securely retains standard electron microscope grid (disk) 3 mm in diameter and absorbs backscattered electrons that otherwise generate spurious X-rays. Since holder inexpensive, dedicated to single specimen when numerous samples examined.

  17. X-ray emission scaling law from a plasma focus with different anode tip materials (Cu, Mo, and W)

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

    Sharif, M.; Ahmad, S.; Zakaullah, M.

    X-ray emission from a 2.3-5.3 kJ Mather-type plasma focus [Phys. Fluids 7, 5 (1964)] employing copper, molybdenum, and tungsten anode tip is studied. Argon is used as a working gas. Characteristic Cu K{alpha} and Mo K-series emission and their ratio to the continuous x-rays are determined. From the variation of the x-ray yield data with filling pressure at different charging voltages, scaling laws are obtained. X-ray pinhole images demonstrate that a significant amount of x-ray emission is from the anode tip. The comparison of the ratio of characteristic to continuum radiation for copper anode with typical x-ray tube data revealsmore » that the contribution of very high energy electron beam from the focus region for x-ray generation through thick target bremsstrahlung mechanism is not significant. Rather, electrons with energy of the order of, or even less than, the charging voltage are responsible for bulk of the x-ray emission.« less

  18. Feasibility study for mega-electron-volt electron beam tomography.

    PubMed

    Hampel, U; Bärtling, Y; Hoppe, D; Kuksanov, N; Fadeev, S; Salimov, R

    2012-09-01

    Electron beam tomography is a promising imaging modality for the study of fast technical processes. But for many technical objects of interest x rays of several hundreds of keV energy are required to achieve sufficient material penetration. In this article we report on a feasibility study for fast electron beam computed tomography with a 1 MeV electron beam. The experimental setup comprises an electrostatic accelerator with beam optics, transmission target, and a single x-ray detector. We employed an inverse fan-beam tomography approach with radiographic projections being generated from the linearly moving x-ray source. Angular projections were obtained by rotating the object.

  19. 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

  20. Ultrafast Independent N-H and N-C Bond Deformation Investigated with Resonant Inelastic X-Ray Scattering

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

    Eckert, Sebastian; Norell, Jesper; Miedema, Piter S.

    Here, the femtosecond excited-state dynamics following resonant photoexcitation enable the selective deformation of N-H and N-C chemical bonds in 2-thiopyridone in aqueous solution with optical or X-ray pulses. In combination with multiconfigurational quantum-chemical calculations, the orbital-specific electronic structure and its ultrafast dynamics accessed with resonant inelastic X-ray scattering at the N 1s level using synchrotron radiation and the soft X-ray free-electron laser LCLS provide direct evidence for this controlled photoinduced molecular deformation and its ultrashort timescale.

  1. Ultrafast Independent N-H and N-C Bond Deformation Investigated with Resonant Inelastic X-Ray Scattering

    DOE PAGES

    Eckert, Sebastian; Norell, Jesper; Miedema, Piter S.; ...

    2017-04-04

    Here, the femtosecond excited-state dynamics following resonant photoexcitation enable the selective deformation of N-H and N-C chemical bonds in 2-thiopyridone in aqueous solution with optical or X-ray pulses. In combination with multiconfigurational quantum-chemical calculations, the orbital-specific electronic structure and its ultrafast dynamics accessed with resonant inelastic X-ray scattering at the N 1s level using synchrotron radiation and the soft X-ray free-electron laser LCLS provide direct evidence for this controlled photoinduced molecular deformation and its ultrashort timescale.

  2. Joule heating and runaway electron acceleration in a solar flare

    NASA Technical Reports Server (NTRS)

    Holman, Gordon D.; Kundu, Mukul R.; Kane, Sharad R.

    1989-01-01

    The hard and soft x ray and microwave emissions from a solar flare (May 14, 1980) were analyzed and interpreted in terms of Joule heating and runaway electron acceleration in one or more current sheets. It is found that all three emissions can be generated with sub-Dreicer electric fields. The soft x ray emitting plasma can only be heated by a single current sheet if the resistivity in the sheet is well above the classical, collisional resistivity of 10(exp 7) K, 10(exp 11)/cu cm plasma. If the hard x ray emission is from thermal electrons, anomalous resistivity or densities exceeding 3 x 10(exp 12)/cu cm are required. If the hard x ray emission is from nonthermal electrons, the emissions can be produced with classical resistivity in the current sheets if the heating rate is approximately 4 times greater than that deduced from the soft x ray data (with a density of 10(exp 10)/cu cm in the soft x ray emitting region), if there are at least 10(exp 4) current sheets, and if the plasma properties in the sheets are characteristic of the superhot plasma observed in some flares by Lin et al., and with Hinotori. Most of the released energy goes directly into bulk heating, rather than accelerated particles.

  3. Effect of enhanced x-ray flux on the ionosphere over Cyprus during solar flares

    NASA Astrophysics Data System (ADS)

    Mostafa, Md. Golam; Haralambous, Haris

    2015-06-01

    In this work we study the effect of solar flares on the ionosphere over Cyprus. Solar flares are impulsive solar activity events usually coupled with Coronal Mass Ejection (CME). The arrival and the subsequent impact of solar flares on geospace, following an eruption on the Sun's surface is almost immediate (around 9 min) whereas the impact of CMEs is rather delayed (2-3 days) as the former is based on X-ray radiation whereas the latter phenomenon is related with particles and magnetic fields travelling at lower speeds via the Solar Wind. The penetration of X-rays down to the Dregion following such an event enhances the electron density. This increase can be monitored by ionosondes, which measure the electron density up to the maximum electron density NmF2. The significance of this increase lies on the increase of signal absorption causing limited window of operating frequencies for HF communications. In this study the effect of enhanced X-ray flux on the ionosphere over Cyprus during solar flares has been investigated. To establish the correlation and extent of impact on different layers, data of X-ray intensity from Geostationary Operational Environmental Satellite (GOES) and ionospheric characteristics (D & F layer) over Nicosia station (35° N, 33° E) were examined for all solar flares during the period 2011-2014. The analysis revealed a positive and good correlation between frequency of minimum reflection, fmin and X-ray intensity for D layer demonstrating that X-rays play a dominant role in the ionization of lower ionosphere. Hence, X-ray flux can be used as a good proxy for studying the solar flare effects on lower ionosphere. The correlation coefficient between maximum electron density of F layer, NmF2 and X-ray intensity was found to be poor.

  4. Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

    DOE PAGES

    Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; ...

    2012-11-05

    The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as wellmore » as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ 1,3 XES spectra of Mn II and Mn 2 III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. Furthermore, the technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II.« less

  5. Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

    PubMed Central

    Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Lassalle-Kaiser, Benedikt; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Hellmich, Julia; Glöckner, Carina; Echols, Nathaniel; Sierra, Raymond G.; Schafer, Donald W.; Sellberg, Jonas; Kenney, Christopher; Herbst, Ryan; Pines, Jack; Hart, Philip; Herrmann, Sven; Grosse-Kunstleve, Ralf W.; Latimer, Matthew J.; Fry, Alan R.; Messerschmidt, Marc M.; Miahnahri, Alan; Seibert, M. Marvin; Zwart, Petrus H.; White, William E.; Adams, Paul D.; Bogan, Michael J.; Boutet, Sébastien; Williams, Garth J.; Zouni, Athina; Messinger, Johannes; Glatzel, Pieter; Sauter, Nicholas K.; Yachandra, Vittal K.; Yano, Junko; Bergmann, Uwe

    2012-01-01

    The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as well as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ1,3 XES spectra of MnII and Mn2III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. The technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II. PMID:23129631

  6. X-ray comb generation from nuclear-resonance-stabilized x-ray free-electron laser oscillator for fundamental physics and precision metrology

    DOE PAGES

    Adams, B.  W.; Kim, K. -J.

    2015-03-31

    An x-ray free-electron laser oscillator (XFELO) is a next-generation x-ray source, similar to free-electron laser oscillators at VUV and longer wavelengths but using crystals as high-reflectivity x-ray mirrors. Each output pulse from an XFELO is fully coherent with high spectral purity. The temporal coherence length can further be increased drastically, from picoseconds to microseconds or even longer, by phase-locking successive XFELO output pulses, using the narrow nuclear resonance lines of nuclei such as ⁵⁷Fe as a reference. We show that the phase fluctuation due to the seismic activities is controllable and that due to spontaneous emission is small. The fluctuationmore » of electron-bunch spacing contributes mainly to the envelope fluctuation but not to the phase fluctuation. By counting the number of standing-wave maxima formed by the output of the nuclear-resonance-stabilized (NRS) XFELO over an optically known length, the wavelength of the nuclear resonance can be accurately measured, possibly leading to a new length or frequency standard at x-ray wavelengths. A NRS-XFELO will be an ideal source for experimental x-ray quantum optics as well as other fundamental physics. The technique can be refined for other, narrower resonances such as ¹⁸¹Ta or ⁴⁵Sc.« less

  7. Analysis of the Relationship Between the Solar X-Ray Radiation Intensity and the D-Region Electron Density Using Satellite and Ground-Based Radio Data

    NASA Astrophysics Data System (ADS)

    Nina, Aleksandra; Čadež, Vladimir M.; Bajčetić, Jovan; Mitrović, Srdjan T.; Popović, Luka Č.

    2018-04-01

    Increases in the X-ray radiation that is emitted during a solar X-ray flare induce significant changes in the ionospheric D region. Because of the numerous complex processes in the ionosphere and the characteristics of the radiation and plasma, the causal-consequential relationship between the X-ray radiation and ionospheric parameters is not easily determined. In addition, modeling the ionospheric D-region plasma parameters is very difficult because of the lack of data for numerous time- and space-dependent physical quantities. In this article we first give a qualitative analysis of the relationship between the electron density and the recorded solar X-ray intensity. After this, we analyze the differences in the relationships between the D-region response and various X-ray radiation properties. The quantitative study is performed for data observed on 5 May 2010 in the time period between 11:40 UT - 12:40 UT when the GOES 14 satellite detected a considerable X-ray intensity increase. Modeling the electron density is based on characteristics of the 23.4 kHz signal emitted in Germany and recorded by the receiver in Serbia.

  8. Simulations of Beam Optics and Bremsstrahlung for High Intensity and Brightness Channeling Radiation

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

    Hyun, J.; Piot, P.; Sen, T.

    2018-04-12

    This paper presents X-ray spectra of channeling radiation expected at the FAST (Fermi Accelerator Science and Technology) facility in Fermilab. Our purpose is to produce high brightness quasi-monochromatic X-rays in an energy range from 40 keV to 110 keV. We will use a diamond crystal and low emittance electrons with an energy of around 43 MeV. The quality of emitted X-rays depends on parameters of the electron beam at the crystal. We present simulations of the beam optics for high brightness and high yield operations for a range of bunch charges. We estimate the X-ray spectra including bremsstrahlung background. Wemore » discuss how the electron beam distributions after the diamond crystal are affected by channeling. We discuss an X-ray detector system to avoid pile-up effects during high charge operations.« less

  9. RHEED-TRAXS as a tool for in-situ stoichiometry control.

    NASA Astrophysics Data System (ADS)

    Chandril, Sandeep; Keenan, Cameron; Myers, Thomas; Lederman, David

    2008-03-01

    RHEED-total reflection x-ray spectroscopy (-TRAXS) is an in-situ chemical and structural characterization technique which is highly surface sensitive. This consists of a grazing-angle electron beam from which characteristic x-rays from the sample are measured also at grazing angles. We have demonstrated that monolayer sensitivity in Y and Mn films on GaN can be achieved. We have also developed a theoretical model for the angular dependence of the x-ray Kα peaks for the thin films, based on Parratt's formalism for x-ray reflectivity and the electron trajectory simulation software CASINO, to correct for grazing angle electron beam as a source for x-rays. As the angular dependence is highly dependent upon the film thickness and the smoothness of the film, it can be used to determine the deposition rate of individual elements as well as the interface chemical roughness

  10. Thick-target bremsstrahlung interpretation of short time-scale solar hard X-ray features

    NASA Technical Reports Server (NTRS)

    Emslie, A. G.

    1983-01-01

    Steady-state analyses of bremsstrahlung hard X-ray production in solar flares are appropriate only if the lifetime of the high energy electrons in the X-ray source is much shorter than the duration of the observed X-ray burst. For a thick-target nonthermal model, this implies that a full time-dependent analysis is required when the duration of the burst is comparable to the collisional lifetime of the injected electrons, in turn set by the lengths and densities of the flaring region. In this paper we present the results of such a time-dependent analysis, and we point out that the intrinsic temporal signature of the thick-target production mechanism, caused by the finite travel time of the electrons through the target, may indeed rule out such a mechanism for extremely short duration hard X-ray events.

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

    Anisimov, Petr Mikhaylovich

    Classical 1D X-ray Free Electron Laser (X-ray FEL) theory has stood the test of time by guiding FEL design and development prior to any full-scale analysis. Future X-ray FELs and inverse-Compton sources, where photon recoil approaches an electron energy spread value, push the classical theory to its limits of applicability. After substantial efforts by the community to find what those limits are, there is no universally agreed upon quantum approach to design and development of future X-ray sources. We offer a new approach to formulate the quantum theory for 1D X-ray FELs that has an obvious connection to the classicalmore » theory, which allows for immediate transfer of knowledge between the two regimes. In conclusion, we exploit this connection in order to draw quantum mechanical conclusions about the quantum nature of electrons and generated radiation in terms of FEL variables.« less

  12. Simulations of Beam Optics and Bremsstrahlung for High Intensity and Brightness Channeling Radiation

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

    Hyun, J.; Piot, P.; Sen, T.

    This paper presents X-ray spectra of channeling radiation expected at the FAST (Fermi Accelerator Science and Technology) facility in Fermilab. Our purpose is to produce high brightness quasi-monochromatic X-rays in an energy range from 40 keV to 110 keV. We will use a diamond crystal and low emittance electrons with an energy of around 43 MeV. The quality of emitted X-rays depends on parameters of the electron beam at the crystal. We present simulations of the beam optics for high brightness and high yield operations for a range of bunch charges. We estimate the X-ray spectra including bremsstrahlung background. Wemore » discuss how the electron beam distributions after the diamond crystal are affected by channeling. Here, we discuss an X-ray detector system to avoid pile-up effects during high charge operations.« less

  13. Simulations of Beam Optics and Bremsstrahlung for High Intensity and Brightness Channeling Radiation

    DOE PAGES

    Hyun, J.; Piot, P.; Sen, T.

    2018-06-14

    This paper presents X-ray spectra of channeling radiation expected at the FAST (Fermi Accelerator Science and Technology) facility in Fermilab. Our purpose is to produce high brightness quasi-monochromatic X-rays in an energy range from 40 keV to 110 keV. We will use a diamond crystal and low emittance electrons with an energy of around 43 MeV. The quality of emitted X-rays depends on parameters of the electron beam at the crystal. We present simulations of the beam optics for high brightness and high yield operations for a range of bunch charges. We estimate the X-ray spectra including bremsstrahlung background. Wemore » discuss how the electron beam distributions after the diamond crystal are affected by channeling. Here, we discuss an X-ray detector system to avoid pile-up effects during high charge operations.« less

  14. The Focusing Optics X-ray Solar Imager (FOXSI) sounding rocket, first flight

    NASA Astrophysics Data System (ADS)

    Christe, Steven; Glesener, L.; Ishikawa, S.; Ramsey, B.; Takahashi, T.; Watanabe, S.; Saito, S.; Lin, R. P.; Krucker, S.

    2013-07-01

    Understanding electron acceleration in solar flares requires X-ray studies with greater sensitivity and dynamic range than are available with current solar hard X-ray observers (i.e. the RHESSI spacecraft). RHESSI employs an indirect Fourier imaging method that is intrinsically limited in dynamic range and therefore can rarely image faint coronal flare sources in the presence of bright footpoints. With greater sensitivity and dynamic range, electron acceleration sites in the corona could be studied in great detail. Both these capabilities can be advanced by the use of direct focusing optics. The recently flown Focusing Optics X-ray Solar Imager (FOXSI) sounding rocket payload demonstrates the feasibility and usefulness of hard X-ray focusing optics for observations of solar hard X-rays. FOXSI features grazing-incidence replicated nickel optics made by the NASA Marshall Space Flight Center and fine-pitch silicon strip detectors developed by the Astro-H team at JAXA/ISAS. FOXSI flew successfully on November 2, 2012, producing images and spectra of a microflare and performing a search for nonthermal emission (4-15 keV) from nanoflares in the quiet Sun. Nanoflares are a candidate for providing the required energy to heat the solar corona to its high temperature of a few million degrees. A future satellite version of FOXSI, featuring similar optics and detectors, could make detailed observations of hard X-rays from flare-accelerated electrons, identifying and characterizing particle acceleration sites and mapping out paths of energetic electrons as they leave these sites and propagate throughout the solar corona.Abstract (2,250 Maximum Characters): Understanding electron acceleration in solar flares requires X-ray studies with greater sensitivity and dynamic range than are available with current solar hard X-ray observers (i.e. the RHESSI spacecraft). RHESSI employs an indirect Fourier imaging method that is intrinsically limited in dynamic range and therefore can rarely image faint coronal flare sources in the presence of bright footpoints. With greater sensitivity and dynamic range, electron acceleration sites in the corona could be studied in great detail. Both these capabilities can be advanced by the use of direct focusing optics. The recently flown Focusing Optics X-ray Solar Imager (FOXSI) sounding rocket payload demonstrates the feasibility and usefulness of hard X-ray focusing optics for observations of solar hard X-rays. FOXSI features grazing-incidence replicated nickel optics made by the NASA Marshall Space Flight Center and fine-pitch silicon strip detectors developed by the Astro-H team at JAXA/ISAS. FOXSI flew successfully on November 2, 2012, producing images and spectra of a microflare and performing a search for nonthermal emission (4-15 keV) from nanoflares in the quiet Sun. Nanoflares are a candidate for providing the required energy to heat the solar corona to its high temperature of a few million degrees. A future satellite version of FOXSI, featuring similar optics and detectors, could make detailed observations of hard X-rays from flare-accelerated electrons, identifying and characterizing particle acceleration sites and mapping out paths of energetic electrons as they leave these sites and propagate throughout the solar corona.

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

    Adhikari, R., E-mail: rajdeep.adhikari@jku.at; Capuzzo, G.; Bonanni, A., E-mail: alberta.bonanni@jku.at

    Polarization induced degenerate n-type doping with electron concentrations up to ∼10{sup 20 }cm{sup −3} is achieved in graded Al{sub x}Ga{sub 1−x}N layers (x: 0% → 37%) grown on unintentionally doped and on n-doped GaN:Si buffer/reservoir layers by metal organic vapor phase epitaxy. High resolution x-ray diffraction, transmission electron microscopy, and electron dispersive x-ray spectroscopy confirm the gradient in the composition of the Al{sub x}Ga{sub 1−x}N layers, while Hall effect studies reveal the formation of a three dimensional electron slab, whose conductivity can be adjusted through the GaN(:Si) buffer/reservoir.

  16. Predicted TeV Gamma-ray Spectra and Images of Shell Supernova Remnants

    NASA Astrophysics Data System (ADS)

    Reynolds, S. P.

    1999-04-01

    One supernova remnant, SN 1006, is now known to produce synchrotron X-rays (Koyama et al., 1995, Nature, 378, 255), requiring 100 TeV electrons. SN 1006 has also been seen in TeV gamma rays (Tanimori et al., 1998, ApJ, 497, L25), almost certainly due to cosmic-microwave-background photons being upscattered by those same electrons. Other young supernova remnants should also produce high-energy electrons, even if their X-ray synchrotron emission is swamped by conventional thermal X-ray emission. Upper limits to the maximum energy of shock-accelerated electrons can be found for those remnants by requiring that their synchrotron spectrum steepen enough to fall below observed thermal X-rays (Reynolds and Keohane 1999, ApJ, submitted). For those upper-limit spectra, I present predicted TeV inverse-Compton spectra and images for assumed values of the mean remnant magnetic field. Ground-based TeV gamma-ray observations of remnants may be able to put even more severe limits on the presence of highly energetic electrons in remnants, raising problems for conventional theories of galactic cosmic-ray production in supernova remnants. Detections will immediately confirm that SN 1006 is not alone, and will give mean remnant magnetic field strengths.

  17. Symposium LL: Nanowires--Synthesis Properties Assembly and Application

    DTIC Science & Technology

    2010-09-10

    dedicated hard x - ray microscopy beamline is operated in partnership with the Advanced Photon Source to provide fluorescence, diffraction, and...characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X - ray diffraction (XRD) measurements, proving it to be...Investigation of Preferred Growth Direction of GaN Nanorods by Synchrotron X - ray Reciprocal Space Mapping. Yuri Sohn1, Sanghwa Lee1, Chinkyo Kim1 and Dong

  18. Effect of insulator sleeve material on the x-ray emission from a plasma focus device

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

    Hussain, S.; Badar, M. A.; Shafiq, M.

    The effect of insulator sleeve material on x-ray emission from a 2.3 kJ Mather type plasma focus device operated in argon-hydrogen mixture is investigated. The time and space resolved x-ray emission characteristics are studied by using a three channel p-i-n diode x-ray spectrometer and a multipinhole camera. The x-ray emission depends on the volumetric ratio of argon-hydrogen mixture as well as the filling pressure and the highest x-ray emission is observed for a volumetric ratio 40% Ar to 60%H{sub 2} at 2.5 mbar filling pressure. The fused silica insulator sleeve produces the highest x-ray emission whereas nonceramic insulator sleeves suchmore » as nylon, Perspex, or Teflon does not produce focus or x-rays. The pinhole images of the x-ray emitting zones reveal that the contribution of the Cu K{alpha} line is weak and plasma x-rays are intense. The highest plasma electron temperature is estimated to be 3.3 and 3.6 keV for Pyrex glass and fused silica insulator sleeves, respectively. It is speculated that the higher surface resistivity of fused silica is responsible for enhanced x-ray emission and plasma electron temperature.« less

  19. Compact X-ray sources: X-rays from self-reflection

    NASA Astrophysics Data System (ADS)

    Mangles, Stuart P. D.

    2012-05-01

    Laser-based particle acceleration offers a way to reduce the size of hard-X-ray sources. Scientists have now developed a simple scheme that produces a bright flash of hard X-rays by using a single laser pulse both to generate and to scatter an electron beam.

  20. Hard X-ray emission from the solar corona

    NASA Astrophysics Data System (ADS)

    Krucker, S.; Battaglia, M.; Cargill, P. J.; Fletcher, L.; Hudson, H. S.; MacKinnon, A. L.; Masuda, S.; Sui, L.; Tomczak, M.; Veronig, A. L.; Vlahos, L.; White, S. M.

    2008-10-01

    This review surveys hard X-ray emissions of non-thermal electrons in the solar corona. These electrons originate in flares and flare-related processes. Hard X-ray emission is the most direct diagnostic of electron presence in the corona, and such observations provide quantitative determinations of the total energy in the non-thermal electrons. The most intense flare emissions are generally observed from the chromosphere at footpoints of magnetic loops. Over the years, however, many observations of hard X-ray and even γ-ray emission directly from the corona have also been reported. These coronal sources are of particular interest as they occur closest to where the electron acceleration is thought to occur. Prior to the actual direct imaging observations, disk occultation was usually required to study coronal sources, resulting in limited physical information. Now RHESSI has given us a systematic view of coronal sources that combines high spatial and spectral resolution with broad energy coverage and high sensitivity. Despite the low density and hence low bremsstrahlung efficiency of the corona, we now detect coronal hard X-ray emissions from sources in all phases of solar flares. Because the physical conditions in such sources may differ substantially from those of the usual “footpoint” emission regions, we take the opportunity to revisit the physics of hard X-radiation and relevant theories of particle acceleration.

  1. Relative merits and limiting factors for x-ray and electron microscopy of thick, hydrated organic materials

    DOE PAGES

    Du, Ming; Jacobsen, Chris

    2017-10-07

    Electron and x-ray microscopes allow one to image the entire, unlabeled structure of hydrated materials at a resolution well beyond what visible light microscopes can achieve. However, both approaches involve ionizing radiation, so that radiation damage must be considered as one of the limits to imaging. Drawing upon earlier work, we describe here a unified approach to estimating the image contrast (and thus the required exposure and corresponding radiation dose) in both x-ray and electron microscopy. This approach accounts for factors such as plural and inelastic scattering, and (in electron microscopy) the use of energy filters to obtain so-called "zeromore » loss" images. As expected, it shows that electron microscopy offers lower dose for specimens thinner than about 1 mu m (such as for studies of macromolecules, viruses, bacteria and archaebacteria, and thin sectioned material), while x-ray microscopy offers superior characteristics for imaging thicker specimen such as whole eukaryotic cells, thick-sectioned tissues, and organs. The required radiation dose scales strongly as a function of the desired spatial resolution, allowing one to understand the limits of live and frozen hydrated specimen imaging. Lastly, we consider the factors limiting x-ray microscopy of thicker materials, suggesting that specimens as thick as a whole mouse brain can be imaged with x-ray microscopes without significant image degradation should appropriate image reconstruction methods be identified.« less

  2. Relative merits and limiting factors for x-ray and electron microscopy of thick, hydrated organic materials

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

    Du, Ming; Jacobsen, Chris

    Electron and x-ray microscopes allow one to image the entire, unlabeled structure of hydrated materials at a resolution well beyond what visible light microscopes can achieve. However, both approaches involve ionizing radiation, so that radiation damage must be considered as one of the limits to imaging. Drawing upon earlier work, we describe here a unified approach to estimating the image contrast (and thus the required exposure and corresponding radiation dose) in both x-ray and electron microscopy. This approach accounts for factors such as plural and inelastic scattering, and (in electron microscopy) the use of energy filters to obtain so-called "zeromore » loss" images. As expected, it shows that electron microscopy offers lower dose for specimens thinner than about 1 mu m (such as for studies of macromolecules, viruses, bacteria and archaebacteria, and thin sectioned material), while x-ray microscopy offers superior characteristics for imaging thicker specimen such as whole eukaryotic cells, thick-sectioned tissues, and organs. The required radiation dose scales strongly as a function of the desired spatial resolution, allowing one to understand the limits of live and frozen hydrated specimen imaging. Lastly, we consider the factors limiting x-ray microscopy of thicker materials, suggesting that specimens as thick as a whole mouse brain can be imaged with x-ray microscopes without significant image degradation should appropriate image reconstruction methods be identified.« less

  3. Simultaneous SMM flat crystal spectrometer and Very Large Array observations of solar active regions

    NASA Technical Reports Server (NTRS)

    Lang, Kenneth R.; Willson, Robert F.; Smith, Kermit L.; Strong, Keith T.

    1987-01-01

    High-resolution images of the quiescent emission from two solar active regions at 20 cm (VLA) and soft X-ray (SMM FCS) wavelengths are compared. There are regions where the X-ray coronal loops have been completely imaged at 20 cm wavelength. In other regions, the X-ray radiation was detected without detectable 20 cm radiation, and vice versa. The X-ray data were used to infer average electron temperatures of about 3-million K and average electron densities of about 2.5 x 10 to the 9th/cu cm for the X-ray emitting plasma in the two active regions. The thermal bremsstrahlung of the X-ray emitting plasma is optically thin at 20 cm wavelength. The 20 cm brightness temperatures were always less than T(e), which is consistent with optically thin bremsstrahlung. The low T(B) can be explained if a higher, cooler plasma covers the hotter X-ray emitting plasma. Thermal gyroresonance radiation must account for the intense 20 cm radiation near and above sunspots where no X-ray radiation is detected.

  4. X-band RF gun and linac for medical Compton scattering X-ray source

    NASA Astrophysics Data System (ADS)

    Dobashi, Katsuhito; Uesaka, Mitsuru; Fukasawa, Atsushi; Sakamoto, Fumito; Ebina, Futaro; Ogino, Haruyuki; Urakawa, Junji; Higo, Toshiyasu; Akemoto, Mitsuo; Hayano, Hitoshi; Nakagawa, Keiichi

    2004-12-01

    Compton scattering hard X-ray source for 10-80 keV are under construction using the X-band (11.424 GHz) electron linear accelerator and YAG laser at Nuclear Engineering Research laboratory, University of Tokyo. This work is a part of the national project on the development of advanced compact medical accelerators in Japan. National Institute for Radiological Science is the host institute and U.Tokyo and KEK are working for the X-ray source. Main advantage is to produce tunable monochromatic hard (10-80 keV) X-rays with the intensities of 108-1010 photons/s (at several stages) and the table-top size. Second important aspect is to reduce noise radiation at a beam dump by adopting the deceleration of electrons after the Compton scattering. This realizes one beamline of a 3rd generation SR source at small facilities without heavy shielding. The final goal is that the linac and laser are installed on the moving gantry. We have designed the X-band (11.424 GHz) traveling-wave-type linac for the purpose. Numerical consideration by CAIN code and luminosity calculation are performed to estimate the X-ray yield. X-band thermionic-cathode RF-gun and RDS(Round Detuned Structure)-type X-band accelerating structure are applied to generate 50 MeV electron beam with 20 pC microbunches (104) for 1 microsecond RF macro-pulse. The X-ray yield by the electron beam and Q-switch Nd:YAG laser of 2 J/10 ns is 107 photons/RF-pulse (108 photons/sec at 10 pps). We design to adopt a technique of laser circulation to increase the X-ray yield up to 109 photons/pulse (1010 photons/s). 50 MW X-band klystron and compact modulator have been constructed and now under tuning. The construction of the whole system has started. X-ray generation and medical application will be performed in the early next year.

  5. Talbot-Lau x-ray deflectometer electron density diagnostic for laser and pulsed power high energy density plasma experiments (invited)

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

    Valdivia, M. P., E-mail: mpvaldivia@pha.jhu.edu; Stutman, D.; Stoeckl, C.

    2016-11-15

    Talbot-Lau X-ray deflectometry (TXD) has been developed as an electron density diagnostic for High Energy Density (HED) plasmas. The technique can deliver x-ray refraction, attenuation, elemental composition, and scatter information from a single Moiré image. An 8 keV Talbot-Lau interferometer was deployed using laser and x-pinch backlighters. Grating survival and electron density mapping were demonstrated for 25–29 J, 8–30 ps laser pulses using copper foil targets. Moiré pattern formation and grating survival were also observed using a copper x-pinch driven at 400 kA, ∼1 kA/ns. These results demonstrate the potential of TXD as an electron density diagnostic for HED plasmas.

  6. Variable soft X-ray excesses in active galactic nuclei from nonthermal electron-positron pair cascades

    NASA Technical Reports Server (NTRS)

    Zdziarski, Andrzej A.; Coppi, Paolo S.

    1991-01-01

    In the present study of the formation of steep soft X-ray excesses that are superposed on flatter, hard X-ray power-law spectra in nonthermal electron-positron pair cascade sources, the soft excess in pair-cascade AGN models appears as a steep power law superposed on the tail of the UV bump and the flat nonthermal (hard X-ray) power law. The model-parameter space in which an excess in soft X-rays is visible is ascertained, and the time-variability of soft excesses in pair cascade models is examined. It is established that the parameter space in which soft excesses appear encompasses the range of preferred input parameters for a recently development Compton reflection model of UV and X-ray emission from the central engine of an AGN.

  7. X-ray dense cellular inclusions in the cells of the green alga Chlamydomonas reinhardtii as seen by soft-x-ray microscopy

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

    Stead, A.D.; Ford, T.W.; Page, A.M.

    1997-04-01

    Soft x-rays, having a greater ability to penetrate biological material than electrons, have the potential for producing images of intact, living cells. In addition, by using the so-called {open_quotes}water window{close_quotes} area of the soft x-ray spectrum, a degree of natural contrast is introduced into the image due to differential absorption of the wavelengths by compounds with a high carbon content compared to those with a greater oxygen content. The variation in carbon concentration throughout a cell therefore generates an image which is dependent upon the carbon density within the specimen. Using soft x-ray contact microscopy the authors have previously examinedmore » the green alga Chlamydomonas reinhardtii, and the most prominent feature of the cells are the numerous x-ray absorbing spheres, But they were not seen by conventional transmission electron microscopy. Similar structures have also been reported by the Goettingen group using their cryo transmission x-ray microscope at BESSY. Despite the fact that these spheres appear to occupy up to 20% or more of the cell volume when seen by x-ray microscopy, they are not visible by transmission electron microscopy. Given the difficulties and criticisms associated with soft x-ray contact microscopy, the present study was aimed at confirming the existence of these cellular inclusions and learning more of their possible chemical composition.« less

  8. Study of runaway electrons with Hard X-ray spectrometry of tokamak plasmas

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

    Shevelev, A.; Chugunov, I.; Khilkevitch, E.

    2014-08-21

    Hard-X-ray spectrometry is a tool widely used for diagnostic of runaway electrons in existing tokamaks. In future machines, ITER and DEMO, HXR spectrometry will be useful providing information on runaway electron energy, runaway beam current and its profile during disruption.

  9. Improved EPMA Trace Element Accuracy Using a Matrix Iterated Quantitative Blank Correction

    NASA Astrophysics Data System (ADS)

    Donovan, J. J.; Wark, D. A.; Jercinovic, M. J.

    2007-12-01

    At trace element levels below several hundred PPM, accuracy is more often the limiting factor for EPMA quantification rather than precision. Modern EPMA instruments equipped with low noise detectors, counting electronics and large area analyzing crystals can now routinely achieve sensitivities for most elements in the 10 to 100 PPM levels (or even lower). But due to various sample and instrumental artifacts in the x-ray continuum, absolute accuracy is often the limiting factor for ultra trace element quantification. These artifacts have various mechanisms, but are usually attributed to sample artifacts (e.g., sample matrix absorption edges)1, detector artifacts (e.g., Ar or Xe absorption edges) 2 and analyzing crystal artifacts (extended peak tails preventing accurate determination of the true background and ¡§negative peaks¡¨ or ¡§holes¡¨ in the x-ray continuum). The latter being first described3 by Self, et al. and recently documented for the Ti kÑ in quartz geo-thermometer. 4 Ti (ka) Ti (ka) Ti (ka) Ti (ka) Ti (ka) Si () O () Total Average: -.00146 -.00031 -.00180 .00013 .00240 46.7430 53.2563 99.9983 Std Dev: .00069 .00075 .00036 .00190 .00117 .00000 .00168 .00419 The general magnitude of these artifacts can be seen in the above analyses of Ti ka in a synthetic quartz standard. The values for each spectrometer/crystal vary systematically from ¡V18 PPM to + 24 PPM. The exact mechanism for these continuum ¡§holes¡¨ is not known but may be related to secondary lattice diffraction occurring at certain Bragg angles depending on crystal mounting orientation for non-isometric analyzing crystals5. These x-ray continuum artifacts can produce systematic errors at levels up to 100 PPM or more depending on the particular analytical situation. In order to correct for these inaccuracies, a ¡§blank¡¨ correction has been developed that applies a quantitative correction to the measured x-ray intensities during the matrix iteration, by calculating the intensity contribution from the systematic quantitative offset from a known (usually zero level) blank standard. Preliminary results from this new matrix iterated trace element blank correction demonstrate that systematic errors can be reduced to single digit PPM levels for many situations. 1B.W. Robinson, N.G. Ware and D.G.W. Smith, 1998. "Modern Electron-Microprobe Trace-Element Analysis in Mineralogy". In Cabri, L.J. and Vaughan, D.J., Eds. "Modern Approaches to Ore and Environmental Mineralogy", Short Course 27. Mineralogical Association of Canada, Ottawa 153-180 2Remond, G., Myklebust, R. Fialin, M. Nockolds, C. Phillips, M. Roques-Carmes, C. ¡§Decomposition of Wavelength Dispersive X-ray Spectra¡¨, Journal of Research of the National Institute of Standards and Technology (J. Res. Natl. Inst. Stand. Technol., v. 107, 509-529 (2002) 3Self, P.G., Norrish, K., Milnes, A.R., Graham, J. & Robinson, B.W. (1990): Holes in the Background in XRS. X-ray Spectrom. 19 (2), 59-61 4Wark, DA, and Watson, EB, 2006, TitaniQ: A Titanium-in-Quartz geothermometer: Contributions to Mineralogy and Petrology, 152:743-754, doi: 10.1007/s00410-006-0132-308

  10. AURORAL X-RAYS, COSMIC RAYS, AND RELATED PHENOMENA DURING THE STORM OF FEBRUARY 10-11, 1958

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

    Winckler, J.R.; Peterson, L.; Hoffman, R.

    1959-06-01

    Balloon observations were made during the auroral storm of February 10- 11, 1958, at Minneapolis. Strong x-ray bursts in two groups were detected. The groups appeared coincident with two large magnetic bays, with strong radio noise absorption, and with the passage across the zenith of a very large amount of auroral luminosity. From the x-ray intensity and measured energies, an electron current of 0.6 x 10/sup 6/ electrons /cm/sup 2// scc was present. These electrons ionizing the upper D layer accounted for the increased cosmic noise absorption. The x-rays themselves carried 1000 times less energy than the electrons and couldmore » not provide sufficient ionization for the observed radio absorption. Visual auroral fornis during this storm are reported to have lower borders at thc 200 to 300 km level. There is thus a difficulty in bringing the electrons to the D layer without ani accompanying visible aurora. A cosmic-ray decrease accompanied the storm and was observed to be from 4 to 6% at sea level, 21% in the balloon altitude ionization, and 15% in total energy influx at 55 deg geomagnetic latitude. Compared with the great intensity of the magnetic and auroral phenomena in this storm, the cosmic-ray modulation was not exceptionally large. (auth)« less

  11. Soft X-ray photoemission study of Co2(Cr1-xFex)Ga Heusler compounds

    NASA Astrophysics Data System (ADS)

    Tsunekawa, Masanori; Hattori, Yoshiro; Sekiyama, Akira; Fujiwara, Hidenori; Suga, Shigemasa; Muro, Takayuki; Kanomata, Takeshi; Imada, Shin

    2015-08-01

    We have performed soft X-ray photoemission spectroscopy (SXPES) and X-ray absorption spectroscopy (XAS) of the Co-based Heusler compounds Co2(Cr1-xFex)Ga (x = 0.0, 0.4, and 1.0) in order to study their electronic structures. Band-structure calculation was carried out and compared with the experimental results. SXPES spectra show hν-dependence, revealing the contributions of the Co, Cr, and Fe 3d electronic states in the valence band. The band width observed by the SXPES seems to be narrower than that predicted by the band-structure calculation. XAS spectra depend strongly on the the value of x in Co2(Cr1-xFex)Ga. The electron correlation effects are found to be stronger as x changes from 0.0 to 1.0.

  12. Generation of stable subfemtosecond hard x-ray pulses with optimized nonlinear bunch compression

    DOE PAGES

    Huang, Senlin; Ding, Yuantao; Huang, Zhirong; ...

    2014-12-15

    In this paper, we propose a simple scheme that leverages existing x-ray free-electron laser hardware to produce stable single-spike, subfemtosecond x-ray pulses. By optimizing a high-harmonic radio-frequency linearizer to achieve nonlinear compression of a low-charge (20 pC) electron beam, we obtain a sharp current profile possessing a few-femtosecond full width at half maximum temporal duration. A reverse undulator taper is applied to enable lasing only within the current spike, where longitudinal space charge forces induce an electron beam time-energy chirp. Simulations based on the Linac Coherent Light Source parameters show that stable single-spike x-ray pulses with a duration less thanmore » 200 attoseconds can be obtained.« less

  13. Soft X-ray spectroscopy of transition metal compounds: a theoretical perspective

    NASA Astrophysics Data System (ADS)

    Bokarev, S. I.; Hilal, R.; Aziz, S. G.; Kühn, O.

    2017-01-01

    To date, X-ray spectroscopy has become a routine tool that can reveal highly local and element-specific information on the electronic structure of atoms in complex environments. Here, we report on the development of an efficient and versatile theoretical methodology for the treatment of soft X-ray spectra of transition metal compounds based on the multi-configurational self-consistent field electronic structure theory. A special focus is put on the L-edge photon-in/photon-out and photon-in/electron-out processes, i.e. X-ray absorption, resonant inelastic scattering, partial fluorescence yield, and photoelectron spectroscopy, all treated on the same theoretical footing. The investigated systems range from small prototypical coordination compounds and catalysts to aggregates of biomolecules.

  14. Novel drift structures for silicon and compound semiconductor X-ray and gamma-ray detectors

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

    Patt, B.E.; Iwanczyk, J.S.

    Recently developed silicon- and compound-semiconductor-based drift detector structures have produced excellent performance for charged particles, X-rays, and gamma rays and for low-signal visible light detection. The silicon drift detector (SDD) structures that the authors discuss relate to direct X-ray detectors and scintillation photon detectors coupled with scintillators for gamma rays. Recent designs include several novel features that ensure very low dark current and hence low noise. In addition, application of thin window technology ensures a very high quantum efficiency entrance window on the drift photodetector. The main features of the silicon drift structures for X rays and light detection aremore » very small anode capacitance independent of the overall detector size, low noise, and high throughput. To take advantage of the small detector capacitance, the first stage of the electronics needs to be integrated into the detector anode. In the gamma-ray application, factors other than electronic noise dominate, and there is no need to integrate the electronics into the anode. Thus, a different drift structure is needed in conjunction with a high-Z material. The main features in this case are large active detector volume and electron-only induced signal.« less

  15. X-ray free electron laser: opportunities for drug discovery.

    PubMed

    Cheng, Robert K Y; Abela, Rafael; Hennig, Michael

    2017-11-08

    Past decades have shown the impact of structural information derived from complexes of drug candidates with their protein targets to facilitate the discovery of safe and effective medicines. Despite recent developments in single particle cryo-electron microscopy, X-ray crystallography has been the main method to derive structural information. The unique properties of X-ray free electron laser (XFEL) with unmet peak brilliance and beam focus allow X-ray diffraction data recording and successful structure determination from smaller and weaker diffracting crystals shortening timelines in crystal optimization. To further capitalize on the XFEL advantage, innovations in crystal sample delivery for the X-ray experiment, data collection and processing methods are required. This development was a key contributor to serial crystallography allowing structure determination at room temperature yielding physiologically more relevant structures. Adding the time resolution provided by the femtosecond X-ray pulse will enable monitoring and capturing of dynamic processes of ligand binding and associated conformational changes with great impact to the design of candidate drug compounds. © 2017 The Author(s). Published by Portland Press Limited on behalf of the Biochemical Society.

  16. An upgraded x-ray spectroscopy diagnostic on MST.

    PubMed

    Clayton, D J; Almagri, A F; Burke, D R; Forest, C B; Goetz, J A; Kaufman, M C; O'Connell, R

    2010-10-01

    An upgraded x-ray spectroscopy diagnostic is used to measure the distribution of fast electrons in MST and to determine Z(eff) and the particle diffusion coefficient D(r). A radial array of 12 CdZnTe hard-x-ray detectors measures 10-150 keV Bremsstrahlung from fast electrons, a signature of reduced stochasticity and improved confinement in the plasma. A new Si soft-x-ray detector measures 2-10 keV Bremsstrahlung from thermal and fast electrons. The shaped output pulses from both detector types are digitized and the resulting waveforms are fit with Gaussians to resolve pileup and provide good time and energy resolution. Lead apertures prevent detector saturation and provide a well-known etendue, while lead shielding prevents pickup from stray x-rays. New Be vacuum windows transmit >2 keV x-rays, and additional Al and Be filters are sometimes used to reduce low energy flux for better resolution at higher energies. Measured spectra are compared to those predicted by the Fokker-Planck code CQL3D to deduce Z(eff) and D(r).

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

    Brown, Matthew A.; Redondo, Amaia Beloqui; Duyckaerts, Nicolas

    A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutionsmore » and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.« less

  18. Liquid metal anode x-ray tubes: interesting, but are they useful?

    NASA Astrophysics Data System (ADS)

    Harding, Geoffrey

    2004-10-01

    An analysis is presented of factors affecting the specific loadability (W mm-2 K-1) of electron impact liquid metal anode x-ray sources (LIMAX). It is shown that in general, the limit to loadability is set by energy deposited in the electron window by inelastic electron scattering. Removal of this energy through convection cooling by the liquid metal stream represents the least efficient thermal transport process in LIMAX. As the electron window energy loss is approximately inversely proportional to the electron beam energy, the power loadability of a LIMAX source operated under otherwise constant conditions scales roughly with the square of the tube voltage. A comparison of the loadability of the liquid metal anode x-ray concept to conventional stationary anode x-ray tubes demonstrates the superiority of the former. The utility of LIMAX-based computed tomography in the field of air cargo container inspection is briefly discussed. In particular its characteristics relative to linac-based air cargo container inspection are highlighted: these include a higher contrast-to-noise ratio (CNR); compact radiation shielding and collimation; reduced detector cross-talk; improved image contrast; and the possibility of combining container CT with material-specific alarm resolution capability based on x-ray diffraction tomography.

  19. Characterization of X80 and X100 Microalloyed Pipeline Steel Using Quantitative X-ray Diffraction

    NASA Astrophysics Data System (ADS)

    Wiskel, J. B.; Li, X.; Ivey, D. G.; Henein, H.

    2018-06-01

    Quantitative X-ray diffraction characterization of four (4) X80 and three (3) X100 microalloyed steels was undertaken. The effect of through-thickness position, processing parameters, and composition on the measured crystallite size, microstrain, and J index (relative magnitude of crystallographic texture) was determined. Microstructure analysis using optical microscopy, scanning electron microscopy, transmission electron microscopy, and electron-backscattered diffraction was also undertaken. The measured value of microstrain increased with increasing alloy content and decreasing cooling interrupt temperature. Microstructural features corresponding to crystallite size in the X80 steels were both above and below the detection limit for quantitative X-ray diffraction. The X100 steels consistently exhibited microstructure features below the crystallite size detection limit. The yield stress of each steel increased with increasing microstrain. The increase in microstrain from X80 to X100 is also associated with a change in microstructure from predominantly polygonal ferrite to bainitic ferrite.

  20. A laser-Compton scattering prototype experiment at 100 MeV linac of Shanghai Institute of Applied Physics.

    PubMed

    Luo, W; Xu, W; Pan, Q Y; Cai, X Z; Chen, J G; Chen, Y Z; Fan, G T; Fan, G W; Guo, W; Li, Y J; Liu, W H; Lin, G Q; Ma, Y G; Shen, W Q; Shi, X C; Xu, B J; Xu, J Q; Xu, Y; Zhang, H O; Yan, Z; Yang, L F; Zhao, M H

    2010-01-01

    As a prototype of the Shanghai Laser Electron Gamma Source in the Shanghai Synchrotron Radiation Facility, an x-ray source based on laser-Compton scattering (LCS) has been installed at the terminal of the 100 MeV linac of the Shanghai Institute of Applied Physics. LCS x-rays are generated by interactions between Q-switched Nd:yttrium aluminum garnet laser pulses [with wavelength of 1064 nm and pulse width of 21 ns (full width at half maximum)] and electron bunches [with energy of 108 MeV and pulse width of 0.95 ns (rms)] at an angle of 42 degrees between laser and electron beam. In order to measure the energy spectrum of LCS x-rays, a Si(Li) detector along the electron beam line axis is positioned at 9.8 m away from a LCS chamber. After background subtraction, the LCS x-ray spectrum with the peak energy of 29.1+/-4.4|(stat)+/-2.1|(syst) keV and the peak width (rms) of 7.8+/-2.8|(stat)+/-0.4|(syst) keV is observed. Normally the 100 MeV linac operates with the electron macropulse charge of 1.0 nC/pulse, and the electron and laser collision repetition rate of 20 Hz. Therefore, the total LCS x-ray flux of (5.2+/-2.0) x 10(2) Hz can be achieved.

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