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  1. Category:X-Ray Diffraction (XRD) | Open Energy Information

    Open Energy Info (EERE)

    X-Ray Diffraction (XRD) Jump to: navigation, search GEOTHERMAL ENERGYGeothermal Home Geothermalpower.jpg Looking for the X-Ray Diffraction (XRD) page? For detailed information on...

  2. Portable X-Ray Diffraction (XRD) | Open Energy Information

    Open Energy Info (EERE)

    X-ray powder diffraction, which has traditionally been used in geology, environmental science, material science, and engineering to rapidly identify unknown crystalline...

  3. X-Ray Diffraction (XRD) | Open Energy Information

    Open Energy Info (EERE)

    under investigation. X-ray powder diffraction is widely used in geology, environmental science, material science, and engineering to rapidly identify unknown crystalline substances...

  4. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Biological Imaging by Soft X-Ray Diffraction Microscopy Print Wednesday, 30 November 2005 00:00 Electron and x-ray...

  5. X-Ray Diffraction Microscopy of Magnetic Structures

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    X-Ray Diffraction Microscopy of Magnetic Structures Print science brief icon Scientists working at ALS Beamline 12.0.2.2 have demonstrated a new x-ray technique for producing short-exposure nanoscale images of the magnetic structure of materials. The new method combines aspects of coherent x-ray diffraction, which can determine 3-D charge distributions, and resonant magnetic scattering, which is sensitive to magnetic structures. Physicists have used coherent x-ray diffraction to measure the

  6. X-Ray Diffraction Microscopy of Magnetic Structures

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    X-Ray Diffraction Microscopy of Magnetic Structures Print science brief icon Scientists working at ALS Beamline 12.0.2.2 have demonstrated a new x-ray technique for producing short-exposure nanoscale images of the magnetic structure of materials. The new method combines aspects of coherent x-ray diffraction, which can determine 3-D charge distributions, and resonant magnetic scattering, which is sensitive to magnetic structures. Physicists have used coherent x-ray diffraction to measure the

  7. X-Ray Diffraction Microscopy of Magnetic Structures

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    X-Ray Diffraction Microscopy of Magnetic Structures Print science brief icon Scientists working at ALS Beamline 12.0.2.2 have demonstrated a new x-ray technique for producing short-exposure nanoscale images of the magnetic structure of materials. The new method combines aspects of coherent x-ray diffraction, which can determine 3-D charge distributions, and resonant magnetic scattering, which is sensitive to magnetic structures. Physicists have used coherent x-ray diffraction to measure the

  8. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    methods (see previous highlight, "Demonstration of Coherent X-Ray Diffraction Imaging"). Experimental diffraction data used as input to the difference map algorithm....

  9. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in...

  10. X-Ray Diffraction Microscopy of Magnetic Structures

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    X-Ray Diffraction Microscopy of Magnetic Structures Print science brief icon Scientists working at ALS Beamline 12.0.2.2 have demonstrated a new x-ray technique for producing...

  11. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in ...

  12. X-Ray Diffraction Microscopy of Magnetic Structures

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    X-Ray Diffraction Microscopy of Magnetic Structures Print science brief icon Scientists working at ALS Beamline 12.0.2.2 have demonstrated a new x-ray technique for producing ...

  13. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with nanometer-scale resolution in three dimensions nonperiodic objects that are several microns in size. To fill this gap, the technique of coherent x-ray diffraction imaging now under development takes advantage of the penetrating power of x rays while simultaneously removing the limitations

  14. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with nanometer-scale resolution in three dimensions nonperiodic objects that are several microns in size. To fill this gap, the technique of coherent x-ray diffraction imaging now under development takes advantage of the penetrating power of x rays while simultaneously removing the limitations

  15. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with nanometer-scale resolution in three dimensions nonperiodic objects that are several microns in size. To fill this gap, the technique of coherent x-ray diffraction imaging now under development takes advantage of the penetrating power of x rays while simultaneously removing the limitations

  16. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with nanometer-scale resolution in three dimensions nonperiodic objects that are several microns in size. To fill this gap, the technique of coherent x-ray diffraction imaging now under development takes advantage of the penetrating power of x rays while simultaneously removing the limitations

  17. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with nanometer-scale resolution in three dimensions nonperiodic objects that are several microns in size. To fill this gap, the technique of coherent x-ray diffraction imaging now under development takes advantage of the penetrating power of x rays while simultaneously removing the limitations

  18. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with nanometer-scale resolution in three dimensions nonperiodic objects that are several microns in size. To fill this gap, the technique of coherent x-ray diffraction imaging now under development takes advantage of the penetrating power of x rays while simultaneously removing the limitations

  19. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with nanometer-scale resolution in three dimensions nonperiodic objects that are several microns in size. To fill this gap, the technique of coherent x-ray diffraction imaging now under development takes advantage of the penetrating power of x rays while simultaneously removing the limitations

  20. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with nanometer-scale resolution in three dimensions nonperiodic objects that are several microns in size. To fill this gap, the technique of coherent x-ray diffraction imaging now under development takes advantage of the penetrating power of x rays while simultaneously removing the limitations

  1. Transient x-ray diffraction and its application to materials science and x-ray optics

    SciTech Connect (OSTI)

    Hauer, A.A.; Kopp, R.; Cobble, J.; Kyrala, G.; Springer, R.

    1997-12-01

    Time resolved x-ray diffraction and scattering have been applied to the measurement of a wide variety of physical phenomena from chemical reactions to shock wave physics. Interest in this method has heightened in recent years with the advent of versatile, high power, pulsed x-ray sources utilizing laser plasmas, electron beams and other methods. In this article, we will describe some of the fundamentals involved in time resolved x-ray diffraction, review some of the history of its development, and describe some recent progress in the field. In this article we will emphasize the use of laser-plasmas as the x-ray source for transient diffraction.

  2. X-ray image reconstruction from a diffraction pattern alone

    SciTech Connect (OSTI)

    Marchesini, Stefano

    2015-03-16

    X-ray diffraction pattern of a sample of 50 nm colloidal gold particles, recorded at a wavelength of 2.1 nm.

  3. X-Ray Diffraction Microscopy of Magnetic Structures (Journal...

    Office of Scientific and Technical Information (OSTI)

    Prev Next Title: X-Ray Diffraction Microscopy of Magnetic Structures Authors: Turner, Joshua J. ; Huang, Xiaojing ; Krupin, Oleg ; Seu, Keoki A. ; Parks, Daniel ; Kevan,...

  4. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Biological Imaging by Soft X-Ray Diffraction Microscopy Biological Imaging by Soft X-Ray Diffraction Microscopy Print Wednesday, 30 November 2005 00:00 Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with nanometer-scale resolution in three dimensions nonperiodic objects that are several microns in size. To fill this gap, the technique of coherent x-ray diffraction imaging now under development takes

  5. Note: Electrochemical cell for in operando X-ray diffraction measurements on a conventional X-ray diffractometer

    SciTech Connect (OSTI)

    Hartung, Steffen; Bucher, Nicolas; Bucher, Ramona; Srinivasan, Madhavi

    2015-08-15

    Electrochemical in operando X-ray diffraction (XRD) is a powerful method to analyze structural changes of energy storage materials while inserting/de-inserting charge carriers, such as Li- or Na-ions, into/from a host structure. The design of an XRD in operando cell is presented, which enables the use of thin (6 μm) aluminum foil as X-ray window as a non-toxic alternative to conventional beryllium windows. Owing to the reduced thickness, diffraction patterns and their changes during cycling can be observed with excellent quality, which was demonstrated for two cathode materials for sodium-ion batteries in a half-cell set-up, P2-Na{sub 0.7}MnO{sub 2} and Na{sub 2.55}V{sub 6}O{sub 16} ⋅ 0.6H{sub 2}O.

  6. X-Ray Diffraction Microscopy of Magnetic Structures

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Lensless Imaging of Magnetic Nanostructures Work performed on ALS Beamline 12.0.2.2 Citation: J.J. Turner et al., "X-Ray Diffraction Microscopy of Magnetic Structures," Phys....

  7. X-Ray Diffraction > Analytical Resources > Research > The Energy Materials

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Center at Cornell Analytical Resources In This Section Differential Electrochemical Mass Spectroscopy (DEMS) Electron Microscopy X-Ray Diffraction X-Ray Diffraction

  8. X-ray Diffraction from Membrane Protein Nanocrystals

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    X-ray Diffraction from Membrane Protein Nanocrystals Authors: Hunter, M.S., DePonte, D.P., Shapiro, D.A., Kirian, R.A., Wang, X., Starodub, D., Marchesini, S., Weierstall, U., Doak, R.B., Spence, J.C.H., and Fromme, P. Title: X-ray Diffraction from Membrane Protein Nanocrystals Source: Biophysical Journal Year: 2011 Volume: 100 Pages: 198-206 ABSTRACT: Membrane proteins constitute >30% of the proteins in an average cell, and yet the number of currently known structures of unique membrane

  9. Biological imaging by soft x-ray diffraction microscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Shapiro, D.; Thibault, P.; Beetz, T.; Elser, V.; Howells, M.; Jacobsen, C.; Kirz, J.; Lima, E.; Miao, H.; Neiman, A. M.; et al

    2005-10-25

    We have used the method of x-ray diffraction microscopy to image the complex-valued exit wave of an intact and unstained yeast cell. The images of the freeze-dried cell, obtained by using 750-eV x-rays from different angular orientations, portray several of the cell's major internal components to 30-nm resolution. The good agreement among the independently recovered structures demonstrates the accuracy of the imaging technique. To obtain the best possible reconstructions, we have implemented procedures for handling noisy and incomplete diffraction data, and we propose a method for determining the reconstructed resolution. This work represents a previously uncharacterized application of x-ray diffractionmore » microscopy to a specimen of this complexity and provides confidence in the feasibility of the ultimate goal of imaging biological specimens at 10-nm resolution in three dimensions.« less

  10. X-Ray Diffraction Project Final Report, Fiscal Year 2006

    SciTech Connect (OSTI)

    Dane V. Morgan

    2006-10-01

    An x-ray diffraction diagnostic system was developed for determining real-time shock-driven lattice parameter shifts in single crystals at the gas gun at TA-IV at Sandia National Laboratories (SNL). The signal-to-noise ratio and resolution of the system were measured using imaging plates as the detector and by varying the slit width. This report includes tests of the x-ray diffraction system using a phosphor coupled to a charge-coupled device (CCD) camera by a coherent fiber-optic bundle. The system timing delay was measured with a newly installed transistor-transistor logic (TTL) bypass designed to reduce the x-ray delay time. The axial misalignment of the Bragg planes was determined with respect to the optical axis for a set of eight LiF [lithium fluoride] crystals provided by SNL to determine their suitability for gas gun experiments.

  11. X-ray micro-diffraction studies of heterogeneous interfaces between...

    Office of Scientific and Technical Information (OSTI)

    Article: X-ray micro-diffraction studies of heterogeneous interfaces between cementitious materials and geological formations Citation Details In-Document Search Title: X-ray ...

  12. Serial femtosecond X-ray diffraction of enveloped virus microcrystals

    SciTech Connect (OSTI)

    Lawrence, Robert M.; Conrad, Chelsie E.; Zatsepin, Nadia A.; Grant, Thomas D.; Liu, Haiguang; James, Daniel; Nelson, Garrett; Subramanian, Ganesh; Aquila, Andrew; Hunter, Mark S.; Liang, Mengning; Boutet, Sbastien; Coe, Jesse; Spence, John C. H.; Weierstall, Uwe; Liu, Wei; Fromme, Petra; Cherezov, Vadim; Hogue, Brenda G.

    2015-08-20

    Serial femtosecond crystallography (SFX) using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ~700 diameter. Microcrystals delivered in viscous agarose medium diffracted to ~40 resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is a pertinent step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

  13. Serial femtosecond X-ray diffraction of enveloped virus microcrystals

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Lawrence, Robert M.; Conrad, Chelsie E.; Zatsepin, Nadia A.; Grant, Thomas D.; Liu, Haiguang; James, Daniel; Nelson, Garrett; Subramanian, Ganesh; Aquila, Andrew; Hunter, Mark S.; et al

    2015-08-20

    Serial femtosecond crystallography (SFX) using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ~700 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ~40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is a pertinent step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

  14. Detecting rare, abnormally large grains by x-ray diffraction

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Detecting rare, abnormally large grains by x-ray diffraction - Sandia Energy Energy Search Icon Sandia Home Locations Contact Us Employee Locator Energy & Climate Secure & Sustainable Energy Future Stationary Power Energy Conversion Efficiency Solar Energy Wind Energy Water Power Supercritical CO2 Geothermal Natural Gas Safety, Security & Resilience of the Energy Infrastructure Energy Storage Nuclear Power & Engineering Grid Modernization Battery Testing Nuclear Energy Defense

  15. High resolution x-ray and gamma ray imaging using diffraction...

    Office of Scientific and Technical Information (OSTI)

    High resolution x-ray and gamma ray imaging using diffraction lenses with mechanically bent crystals Title: High resolution x-ray and gamma ray imaging using diffraction lenses ...

  16. Ultrafast resonant soft x-ray diffraction dynamics of the charge...

    Office of Scientific and Technical Information (OSTI)

    Ultrafast resonant soft x-ray diffraction dynamics of the charge density wave in TbTe 3 ... Title: Ultrafast resonant soft x-ray diffraction dynamics of the charge density wave in ...

  17. High-pressure X-ray diffraction, Raman, and computational studies...

    Office of Scientific and Technical Information (OSTI)

    X-ray diffraction, Raman, and computational studies of MgCl2 up to 1 Mbar: Extensive ... Citation Details In-Document Search Title: High-pressure X-ray diffraction, Raman, and ...

  18. X-Ray Diffraction Observations of a Charge-Density-Wave Order...

    Office of Scientific and Technical Information (OSTI)

    X-Ray Diffraction Observations of a Charge-Density-Wave Order in Superconducting Ortho-II ... Citation Details In-Document Search Title: X-Ray Diffraction Observations of a ...

  19. Time-resolved x-ray diffraction across water-ices VI/VII transformatio...

    Office of Scientific and Technical Information (OSTI)

    Conference: Time-resolved x-ray diffraction across water-ices VIVII transformations using dynamic-DAC Citation Details In-Document Search Title: Time-resolved x-ray diffraction ...

  20. High-pressure X-ray diffraction, Raman, and computational studies...

    Office of Scientific and Technical Information (OSTI)

    High-pressure X-ray diffraction, Raman, and computational studies of MgCl2 up to 1 Mbar: ... Citation Details In-Document Search Title: High-pressure X-ray diffraction, Raman, and ...

  1. Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals...

    Office of Scientific and Technical Information (OSTI)

    Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals Citation Details In-Document Search Title: Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals...

  2. High-Energy X-Ray Diffraction Analysis Tool

    Energy Science and Technology Software Center (OSTI)

    2011-11-29

    The functionality of heRXD includes the following: distance and angular calibration and viewing flat-panel detector images used for X-ray diffraction; image (polar) rebinning or "caking"; line position fitting in powder diffraction images; image segmentation or "blob finding"; crystal orentation indesing; and lattice vector refinement. These functionalities encompass a critical set analyzing teh data for high-energy diffraction measurements that are currently performed at synchrotron sources such as the Advanced Photon Source (APS). The software design modularmore » and open source under LGPL. The intent is to provide a common framework and graphical user interface that has the ability to utillize internal as well as external subroutines to provide various optins for performing the fuctionalities listed above. The software will initially be deployed at several national user facilities--including APS, ALS, and CHESS--and then made available for download using a hosting service such as sourceforge.« less

  3. X-Ray Diffraction of Heterogeneous Solid Hydrogen - Oral Presentation

    SciTech Connect (OSTI)

    Levitan, Abraham

    2015-08-24

    Angularly resolved x-ray diffraction at 5.5 keV establishes the structure of a 5 μm diameter solid hydrogen jet, providing a foundation for analysis of hydrogen in a warm dense matter state. The jet was composed of approximately 65% ± 5% HCP and 35% ± 5% FCC by volume with an average crystallite size on the order of hundreds of nanometers. Broadening in the angularly resolved spectrum provided strong evidence for anisotropic strain up to approximately 3 % in the HCP lattice. Finally, we found no evidence for orientational ordering of the crystal domains.

  4. The three dimensional X-ray diffraction technique

    SciTech Connect (OSTI)

    Jensen, D. Juul; Poulsen, H.F.

    2012-10-15

    This introductory tutorial describes the so called 3 dimensional X-ray diffraction (3DXRD) technique, which allows bulk non-destructive structural characterizations of crystalline materials. The motivations and history behind the development of this technique are described and its potentials are sketched. Examples of the use of the technique are given and future trends and developments are suggested. The primary aim of the paper is to give 3DXRD novices an easy introduction to the technique and to describe a way from a dream to reality and new results.

  5. Ultrafast X-Ray Diffraction of Heterogeneous Solid Hydrogen

    SciTech Connect (OSTI)

    Levitan, Abraham

    2015-08-19

    Angularly resolved x-ray diffraction at 5.5 keV establishes the structure of a 5 µm diameter solid hydrogen jet, providing a foundation for analysis of hydrogen in a warm dense matter state. The jet was composed of approximately 65 % ± 5% HCP and 35 % ± 5% FCC by volume with an average crystallite size on the order of hundreds of nanometers. Broadening in the angularly resolved spectrum provided strong evidence for anisotropic strain up to approximately 3 % in the HCP lattice. Finally, we found no evidence for orientational ordering of the crystal domains.

  6. Effects of Plant Cell Wall Matrix Polysaccharides on Bacterial Cellulose Structure Studied with Vibrational Sum Frequency Generation Spectroscopy and X-ray Diffraction

    SciTech Connect (OSTI)

    Park, Yong Bum; Lee, Christopher M; Kafle, Kabindra; Park, Sunkyu; Cosgrove, Daniel; Kim, Seong H

    2014-07-14

    The crystallinity, allomorph content, and mesoscale ordering of cellulose produced by Gluconacetobacter xylinus cultured with different plant cell wall matrix polysaccharides were studied with vibrational sum frequency generation (SFG) spectroscopy and X-ray diffraction (XRD).

  7. Quality experimental and calculated powder x-ray diffraction

    SciTech Connect (OSTI)

    Sullenger, D.B.; Cantrell, J.S.; Beiter, T.A.; Tomlin, D.W.

    1996-08-01

    For several years, we have submitted quality powder XRD patterns to the International Centre for Diffraction Data for inclusion as reference standards in their Powder Diffraction File. The procedure followed is described; examples used are {beta}-UH{sub 3}, {alpha}- BaT{sub 2}, alpha-lithium disilicate ({alpha}-Li{sub 2}Si{sub 2}O{sub 5}), and 2,2`,4,4`,6,6`hexanitroazobenzene-III (HNAB-III).

  8. An image focusing means by using an opaque object to diffract x-rays

    DOE Patents [OSTI]

    Sommargren, Gary E.; Weaver, H. Joseph

    1991-01-01

    The invention provides a method and apparatus for focusing and imaging x-rays. An opaque sphere is used as a diffractive imaging element to diffract x-rays from an object so that the divergent x-ray wavefronts are transformed into convergent wavefronts and are brought to focus to form an image of the object with a large depth of field.

  9. Combining X-ray Absorption and X-ray Diffraction Techniques for in Situ Studies of Chemical Transformations in Heterogeneous Catalysis: Advantages and Limitations

    SciTech Connect (OSTI)

    Frenkel, A.I.; Hanson, J.; Wang, Q.; Marinkovic, N.; Chen, J.G.; Barrio, L.; Si, R.; Lopez Camara, A.; Estrella, A.M.; Rodriguez, J.A.

    2011-08-05

    Recent advances in catalysis instrumentations include synchrotron-based facilities where time-resolved X-ray scattering and absorption techniques are combined in the same in situ or operando experiment to study catalysts at work. To evaluate the advances and limitations of this method, we performed a series of experiments at the new XAFS/XRD instrument in the National Synchrotron Light Source. Nearly simultaneous X-ray diffraction (XRD) and X-ray absorption fine-structure (XAFS) measurements of structure and kinetics of several catalysts under reducing or oxidizing conditions have been performed and carefully analyzed. For CuFe{sub 2}O{sub 4} under reducing conditions, the combined use of the two techniques allowed us to obtain accurate data on kinetics of nucleation and growth of metallic Cu. For the inverse catalyst CuO/CeO{sub 2} that underwent isothermal reduction (with CO) and oxidation (with O{sub 2}), the XAFS data measured in the same experiment with XRD revealed strongly disordered Cu species that went undetected by diffraction. These and other examples emphasize the unique sensitivity of these two complementary methods to follow catalytic processes in the broad ranges of length and time scales.

  10. Combining X-ray Absorption and X-ray Diffraction Techniques for in Situ Studies of Chemical Transformations in Heterogeneous Catalysis:Advantages and Limitations

    SciTech Connect (OSTI)

    A Frenkel; Q Wang; N Marinkovic; J Chen; L Barrio; R Si; A Lopez Camara; A Estella; J Rodriquez; J Hanson

    2011-12-31

    Recent advances in catalysis instrumentations include synchrotron-based facilities where time-resolved X-ray scattering and absorption techniques are combined in the same in situ or operando experiment to study catalysts at work. To evaluate the advances and limitations of this method, we performed a series of experiments at the new XAFS/XRD instrument in the National Synchrotron Light Source. Nearly simultaneous X-ray diffraction (XRD) and X-ray absorption fine-structure (XAFS) measurements of structure and kinetics of several catalysts under reducing or oxidizing conditions have been performed and carefully analyzed. For CuFe{sub 2}O{sub 4} under reducing conditions, the combined use of the two techniques allowed us to obtain accurate data on kinetics of nucleation and growth of metallic Cu. For the inverse catalyst CuO/CeO{sub 2} that underwent isothermal reduction (with CO) and oxidation (with O{sub 2}), the XAFS data measured in the same experiment with XRD revealed strongly disordered Cu species that went undetected by diffraction. These and other examples emphasize the unique sensitivity of these two complementary methods to follow catalytic processes in the broad ranges of length and time scales.

  11. Femtosecond diffractive imaging with a soft-X-ray free-electron...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    from the FLASH soft-X-ray free-electron laser to record a coherent X-ray diffraction ... of 60,000 K. No evidence of sample damage could be seen in the reconstructed image. ...

  12. Variable-metric diffraction crystals for x-ray optics

    SciTech Connect (OSTI)

    Smither, R.K.; Fernandez, P.B. )

    1992-02-01

    A variable-metric (VM) crystal is one in which the spacing between the crystalline planes changes with position in the crystal. This variation can be either parallel to the crystalline planes or perpendicular to the crystalline planes of interest and can be produced by either introducing a thermal gradient in the crystal or by growing a crystal made of two or more elements and changing the relative percentages of the two elements as the crystal is grown. A series of experiments were performed in the laboratory to demonstrate the principle of the variable-metric crystal and its potential use in synchrotron beam lines. One of the most useful applications of the VM crystal is to increase the number of photons per unit bandwidth in a diffracted beam without losing any of the overall intensity. In a normal synchrotron beam line that uses a two-crystal monochromator, the bandwidth of the diffracted photon beam is determined by the vertical opening angle of the beam which is typically 0.10--0.30 mrad or 20--60 arcsec. When the VM crystal approach is applied, the bandwidth of the beam can be made as narrow as the rocking curve of the diffracting crystal, which is typically 0.005--0.050 mrad or 1--10 arcsec. Thus a very large increase of photons per unit bandwidth (or per unit energy) can be achieved through the use of VM crystals. When the VM principle is used with bent crystals, new kinds of x-ray optical elements can be generated that can focus and defocus x-ray beams much like simple lenses where the focal length of the lens can be changed to match its application. Thus both large magnifications and large demagnifications can be achieved as well as parallel beams with narrow bandwidths.

  13. Single-crystal X-ray diffraction at extreme conditions: a review...

    Office of Scientific and Technical Information (OSTI)

    Title: Single-crystal X-ray diffraction at extreme conditions: a review Authors: Ballaran, Tiziana Boffa ; Kurnosov, Alexander ; Trots, Dmytro 1 + Show Author Affiliations ...

  14. X-ray diffraction study of crystalline barium titanate ceramics

    SciTech Connect (OSTI)

    Zali, Nurazila Mat; Mahmood, Che Seman; Mohamad, Siti Mariam; Foo, Choo Thye; Murshidi, Julie Adrianny

    2014-02-12

    In this study, BaTiO{sub 3} ceramics have been prepared via solid-state reaction method. The powders were calcined for 2 hours at different temperatures ranging from 600C to 1200C. Using X-ray diffraction with a Rietveld analysis, the phase formation and crystal structure of the BaTiO{sub 3} powders were studied. Change in crystallite size and tetragonality as a function of calcination temperature were also discussed. It has been found that the formation of pure perovskite phase of BaTiO{sub 3} began at calcination condition of 1000 C for 2 hours. The crystal structure of BaTiO{sub 3} formed is in the tetragonal structure. The second phases of BaCO{sub 3} and TiO{sub 2} existed with calcination temperature below 1000 C. Purity, crystallite size and tetragonality of BaTiO{sub 3} powders were found to increase with increasing calcination temperature.

  15. Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; Lima, Enju; Marchesini, Stefano; Miao, Huijie; Neiman, Aaron M.; Shapiro, David; Steinbrener, Jan; Stewart, Andrew; et al

    2009-11-01

    We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

  16. Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

    SciTech Connect (OSTI)

    Huang Xiaojing; Nelson, Johanna; Lima, Enju; Miao, Huijie; Steinbrener, Jan; Stewart, Andrew; Turner, Joshua J.; Jacobsen, Chris; Kirz, Janos; Marchesini, Stefano; Shapiro, David; Neiman, Aaron M.

    2009-11-06

    We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 deg. C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

  17. X-Ray Diffraction Microscopy of Magnetic Structures

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    This method can be used at any coherent light source, such as x-ray free-electron lasers, where ultra-short pulses would freeze-frame magnetic changes, offering the potential for ...

  18. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Microscopy Print Electron and x-ray microscopes are a valuable tool for both the life and materials sciences, but they are limited in their ability to image with...

  19. Biological Imaging by Soft X-Ray Diffraction Microscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    and angles of x rays scattered from the sample rather than transmitted through it). Shapiro et al. have now chimed in with the first lensless imaging of a sample as complex as a...

  20. Self-terminating diffraction gates femtosecond X-ray nanocrystallograp...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    without the requirement for the pulse to terminate before the onset of sample damage. ... indicate that current X-ray free-electron laser technology5 should enable structural ...

  1. Time-resolved x-ray diffraction across water-ices VI/VII transformatio...

    Office of Scientific and Technical Information (OSTI)

    diffraction across water-ices VIVII transformations using dynamic-DAC Citation Details In-Document Search Title: Time-resolved x-ray diffraction across water-ices VIVII ...

  2. Probing Martensitic Transition in Nitinol Wire: A Comparison of X-ray Diffraction and Other Techniques

    SciTech Connect (OSTI)

    Butler, J.; Tiernan, P.; Tofail, S. A. M.; Ghandi, A. A.

    2011-01-17

    Martensitic to austenite transformation in Nitinol wire can be measured by a number of techniques such as XRD (X-Ray Diffraction), DSC (Differential Scanning Calorimetry), BFR (Bend and Free Recovery) and Vickers indentation recovery. A comparison of results from these varied characterisation techniques is reported here to obtain a greater understanding of the thermal-elastic-structural changes associated with martensitic transformation. The transformation temperatures measured by DSC were found to correspond well with the structural and mechanical information obtained from XRD, BFR and Vickers indent recovery methods. Indent recovery is a relatively new and accurate method of monitoring stress induced martensitic transformations in NiTi and is one of only a few methods of stress inducing martensitic transformation in large scale samples. It is especially useful for NiTi in the as-cast billet form, where tensile testing is impossible. BFR is uniquely popular in the NiTi wire manufacturing sector and is recognised as the most accurate method of measuring the transformation temperature. Here the material is stressed to a representative in-service stress level during the test. No other test uses the shape memory effect for measuring the transformation temperature of NiTi. The results show that the DSC thermogram and XRD diffractogram have a peak overlap which is a common occurrence in NiTi that has been extensively processed. The XRD method further explains the observations in the DSC thermogram and in combination they confirm the transformation temperature.

  3. Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Wang, H.; Kirkham, M. J.; Watkins, T. R.; Payzant, E. A.; Salvador, J. R.; Thompson, A. J.; Sharp, J.; Brown, D.; Miller, D.

    2016-02-17

    N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

  4. Calcination products of gibbsite studied by X-ray diffraction, XPS and solid-state NMR

    SciTech Connect (OSTI)

    Malki, A.; Mekhalif, Z.; Detriche, S.; Fonder, G.; Boumaza, A.; Djelloul, A.

    2014-07-01

    The changes caused by heat treatment of gibbsite powder at 300–1473 K were studied using the X-ray diffraction (XRD), X-ray photoemission (XPS) spectra and {sup 27}Al magic angle spinning nuclear magnetic resonance spectroscopy ({sup 27}Al MAS NMR). XRD analysis indicates that the transformation sequence involves the formation of κ-Al{sub 2}O{sub 3} as an intermediate phase between χ- and α-Al{sub 2}O{sub 3}. The crystallite size of χ-Al{sub 2}O{sub 3} is as small as 10 nm. XPS analysis indicates that the ratio of aluminium atoms to oxygen atoms in χ-Al{sub 2}O{sub 3} and κ-Al{sub 2}O{sub 3} increases, whereas the expected ratio is observed in α-Al{sub 2}O{sub 3}. The percentage of AlO{sub 4} units in the transition aluminas follows the same behaviour as the ratio of Al/O. - Graphical abstract: The percentage of AlO{sub 4} units in transition aluminas follows the same behaviour as the ratio of Al/O. - Highlights: • Calcination products of gibbsite studied by XRD, XPS and solid-state NMR. • The crystallite size of χ-Al{sub 2}O{sub 3} is as small as 10 nm. • The Al/O atomic ratio determined by XPS is larger than 2/3 in χ-Al{sub 2}O{sub 3} and κ-Al{sub 2}O{sub 3}. • The percentage of AlO{sub 4} in the aluminas follows the same behaviour as the Al/O atomic ratio.

  5. Anti-contamination device for cryogenic soft X-ray diffraction microscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; Turner, Joshua; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Jacobsen, Chris

    2011-05-01

    Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

  6. 7 Resolution in Protein 2-Dimentional-Crystal X-Ray Diffraction...

    Office of Scientific and Technical Information (OSTI)

    Journal Article: 7 Resolution in Protein 2-Dimentional-Crystal X-Ray Diffraction at Linac Coherent Light Source Citation Details In-Document Search Title: 7 Resolution in...

  7. DIOPTAS: a program for reduction of two-dimensional X-ray diffraction...

    Office of Scientific and Technical Information (OSTI)

    DIOPTAS: a program for reduction of two-dimensional X-ray diffraction data and data exploration Citation Details In-Document Search Title: DIOPTAS: a program for reduction of ...

  8. Method for improve x-ray diffraction determinations of residual stress in nickel-base alloys

    DOE Patents [OSTI]

    Berman, Robert M.; Cohen, Isadore

    1990-01-01

    A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys which comprises covering part of a predetermined area of the surface of a nickel-base alloy with a dispersion, exposing the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample.

  9. Method for improving x-ray diffraction determinations of residual stress in nickel-base alloys

    DOE Patents [OSTI]

    Berman, R.M.; Cohen, I.

    1988-04-26

    A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys is discussed. Part of a predetermined area of the surface of a nickel-base alloy is covered with a dispersion. This exposes the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose, since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample. 2 figs.

  10. Spectral Resolution for Five-Element, Filtered, X-Ray Detector (XRD) Arrays Using the Methods of Backus and Gilbert

    SciTech Connect (OSTI)

    FEHL,DAVID LEE; BIGGS,F.; CHANDLER,GORDON A.; STYGAR,WILLIAM A.

    2000-01-17

    The generalized method of Backus and Gilbert (BG) is described and applied to the inverse problem of obtaining spectra from a 5-channel, filtered array of x-ray detectors (XRD's). This diagnostic is routinely fielded on the Z facility at Sandia National Laboratories to study soft x-ray photons ({le}2300 eV), emitted by high density Z-pinch plasmas. The BG method defines spectral resolution limits on the system of response functions that are in good agreement with the unfold method currently in use. The resolution so defined is independent of the source spectrum. For noise-free, simulated data the BG approximating function is also in reasonable agreement with the source spectrum (150 eV black-body) and the unfold. This function may be used as an initial trial function for iterative methods or a regularization model.

  11. Measurement of piezoelectric constants of lanthanum-gallium tantalate crystal by X-ray diffraction methods

    SciTech Connect (OSTI)

    Blagov, A. E.; Marchenkov, N. V. Pisarevsky, Yu. V.; Prosekov, P. A.; Kovalchuk, M. V.

    2013-01-15

    A method for measuring piezoelectric constants of crystals of intermediate systems by X-ray quasi-multiple-wave diffraction is proposed and implemented. This technique makes it possible to determine the piezoelectric coefficient by measuring variations in the lattice parameter under an external electric field. This method has been approved, its potential is evaluated, and a comparison with high-resolution X-ray diffraction data is performed.

  12. X-ray diffraction characterization of suspended structures forMEMS applications

    SciTech Connect (OSTI)

    Goudeau, P.; Tamura, N.; Lavelle, B.; Rigo, S.; Masri, T.; Bosseboeuf, A.; Sarnet, T.; Petit, J.-A.; Desmarres, J.-M.

    2005-09-15

    Mechanical stress control is becoming one of the major challenges for the future of micro and nanotechnologies. Micro scanning X-ray diffraction is one of the promising techniques that allows stress characterization in such complex structures at sub micron scales. Two types of MEMS structure have been studied: a bilayer cantilever composed of a gold film deposited on poly-silicon and a boron doped silicon bridge. X-ray diffraction results are discussed in view of numerical simulation experiments.

  13. In-situ X-ray diffraction system using sources and detectors at fixed angular positions

    DOE Patents [OSTI]

    Gibson, David M.; Gibson, Walter M.; Huang, Huapeng

    2007-06-26

    An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

  14. High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stephano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

    2010-04-20

    X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane andmore » freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.« less

  15. High-resolution ab initio three-dimensional x-ray diffraction microscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; Noy, Aleksandr; Hau-Riege, Stefan P.; Cui, Congwu; Howells, Malcolm R.; Rosen, Rachel; He, Haifeng; Spence, John C. H.; et al

    2006-01-01

    Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and largest scattering angles recorded. We demonstrate x-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatialmore » resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.« less

  16. High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

    SciTech Connect (OSTI)

    Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stephano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

    2010-04-20

    X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the ?-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane and freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.

  17. New developments in micro-X-ray diffraction and X-ray absorption spectroscopy for high-pressure research at 16-BM-D at the Advanced Photon Source

    SciTech Connect (OSTI)

    Park, Changyong Popov, Dmitry; Ikuta, Daijo; Lin, Chuanlong; Kenney-Benson, Curtis; Rod, Eric; Bommannavar, Arunkumar; Shen, Guoyin

    2015-07-15

    The monochromator and focusing mirrors of the 16-BM-D beamline, which is dedicated to high-pressure research with micro-X-ray diffraction (micro-XRD) and X-ray absorption near edge structure (XANES) (6-45 keV) spectroscopy, have been recently upgraded. Monochromatic X-rays are selected by a Si (111) double-crystal monochromator operated in an artificial channel-cut mode and focused to 5 μm × 5 μm (FWHM) by table-top Kirkpatrick-Baez type mirrors located near the sample stage. The typical X-ray flux is ∼5 × 10{sup 8} photons/s at 30 keV. The instrumental resolution, Δq/q{sub max}, reaches to 2 × 10{sup −3} and is tunable through adjustments of the detector distance and X-ray energy. The setup is stable and reproducible, which allows versatile application to various types of experiments including resistive heating and cryogenic cooling as well as ambient temperature compression. Transmission XANES is readily combined with micro-XRD utilizing the fixed-exit feature of the monochromator, which allows combined XRD-XANES measurements at a given sample condition.

  18. Multiferroic CuCrO? under high pressure: In situ X-ray diffraction and Raman spectroscopic studies

    SciTech Connect (OSTI)

    Garg, Alka B. Mishra, A. K.; Pandey, K. K.; Sharma, Surinder M.

    2014-10-07

    The compression behavior of delafossite compound CuCrO? has been investigated by in situ x-ray diffraction (XRD) and Raman spectroscopic measurements up to 23.2 and 34 GPa, respectively. X-ray diffraction data show the stability of ambient rhombohedral structure up to ~23 GPa. Material shows large anisotropy in axial compression with c-axis compressibility, ?{sub c} = 1.26 10?(1) GPa? and a-axis compressibility, ?{sub a} = 8.90 10?(6) GPa?. Our XRD data show an irreversible broadening of diffraction peaks. Pressure volume data when fitted to 3rd order Birch-Murnaghan equation of state give the value of bulk modulus, B? = 156.7(2.8) GPa with its pressure derivative, B?{sup } as 5.3(0.5). All the observed vibrational modes in Raman measurements show hardening with pressure. Appearance of a new mode at ~24 GPa indicates the structural phase transition in the compound. Our XRD and Raman results indicate that CuCrO{sub 2} may be transforming to an ordered rocksalt type structure under compression.

  19. In situ laser heating and radial synchrotron x-ray diffraction in a diamond anvil cell

    SciTech Connect (OSTI)

    Kunz, Martin; Caldwell, Wendel A.; Miyagi, Lowell; Wenk, Hans-Rudolf

    2007-06-15

    We report a first combination of diamond anvil cell radial x-ray diffraction with in situ laser heating. The laser-heating setup of ALS beamline 12.2.2 was modified to allow one-sided heating of a sample in a diamond anvil cell with an 80 W yttrium lithium fluoride laser while probing the sample with radial x-ray diffraction. The diamond anvil cell is placed with its compressional axis vertical, and perpendicular to the beam. The laser beam is focused onto the sample from the top while the sample is probed with hard x-rays through an x-ray transparent boron-epoxy gasket. The temperature response of preferred orientation of (Fe,Mg)O is probed as a test experiment. Recrystallization was observed above 1500 K, accompanied by a decrease in stress.

  20. Quantitative determination of mineral composition by powder X-ray diffraction

    DOE Patents [OSTI]

    Pawloski, Gayle A.

    1986-01-01

    An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

  1. Quantitative determination of mineral composition by powder x-ray diffraction

    DOE Patents [OSTI]

    Pawloski, G.A.

    1984-08-10

    An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

  2. X-ray diffraction and EXAFS analysis of materials for lithium-based rechargeable batteries

    SciTech Connect (OSTI)

    Sharkov, M. D., E-mail: mischar@mail.ioffe.ru; Boiko, M. E.; Bobyl, A. V.; Ershenko, E. M.; Terukov, E. I. [Russian Academy of Sciences, Ioffe Physical-Technical Institute (Russian Federation); Zubavichus, Y. V. [National Research Centre Kurchatov Institute (Russian Federation)

    2013-12-15

    Lithium iron phosphate LiFePO{sub 4} (triphylite) and lithium titanate Li{sub 4}Ti{sub 5}O{sub 12} are used as components of a number of active materials in modern rechargeable batteries. Samples of these materials are studied by X-ray diffraction and extended X-ray absorption fine structure (EXAFS) spectroscopy. Hypotheses about the phase composition of the analyzed samples are formulated.

  3. SCANNING ELECTRON MICROSCOPY AND X-RAY DIFFRACTION ANALYSIS OF TANK 18 SAMPLES

    SciTech Connect (OSTI)

    Hay, M.; O'Rourke, P.; Ajo, H.

    2012-03-08

    The F-Area Tank Farm (FTF) Performance Assessment (PA) utilizes waste speciation in the waste release model used in the FTF fate and transport modeling. The waste release modeling associated with the residual plutonium in Tank 18 has been identified as a primary contributor to the Tank 18 dose uncertainty. In order to reduce the uncertainty related to plutonium in Tank 18, a better understanding of the plutonium speciation in the Tank 18 waste (including the oxidation state and stoichiometry) is desired. Savannah River National Laboratory (SRNL) utilized Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD) to analyze Tank 18 samples to provide information on the speciation of plutonium in the waste material. XRD analysis of the Tank 18 samples did not identify any plutonium mineral phases in the samples. These indicates the crystalline mineral phases of plutonium are below the detection limits of the XRD method or that the plutonium phase(s) lack long range order and are present as amorphous or microcrystalline solids. SEM analysis of the Tank 18 samples did locate particles containing plutonium. The plutonium was found as small particles, usually <1 {micro}m but ranging up to several micrometers in diameter, associated with particles of an iron matrix and at low concentration in other elemental matrices. This suggests the plutonium has an affinity for the iron matrix. Qualitatively, the particles of plutonium found in the SEM analysis do not appear to account for all of the plutonium in the sample based on concentrations determined from the chemical analysis of the Tank 18 samples. This suggests that plutonium is also distributed throughout the solids in low concentrations.

  4. Signal-to-noise and radiation exposure considerations in conventional and diffraction x-ray microscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Huang, Xiaojing; Miao, Huijie; Steinbrener, Jan; Nelson, Johanna; Shapiro, David; Stewart, Andrew; Turner, Joshua; Jacobsen, Chris

    2009-01-01

    Using a signal-to-noise ratio estimation based on correlations between multiple simulated images, we compare the dose efficiency of two soft x-ray imaging systems: incoherent brightfield imaging using zone plate optics in a transmission x-ray microscope (TXM), and x-ray diffraction microscopy (XDM) where an image is reconstructed from the far-field coherent diffraction pattern. In XDM one must computationally phase weak diffraction signals; in TXM one suffers signal losses due to the finite numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution imagesmore » using fewer photons. As a result, this can be an important advantage for studying radiation-sensitive biological and soft matter specimens.« less

  5. Coherent x-ray diffraction imaging of paint pigmentparticles by scanning a phase plate modulator

    SciTech Connect (OSTI)

    Chu Y. S.; Chen B.; Zhang F.; Berenguer F.; Bean R.; Kewish C.; Vila-Comamala J.; Rodenburg J.; Robinson I.

    2011-10-19

    We have implemented a coherent x-ray diffraction imaging technique that scans a phase plate to modulate wave-fronts of the x-ray beam transmitted by samples. The method was applied to measure a decorative alkyd paint containing iron oxide red pigment particles. By employing an iterative algorithm for wave-front modulation phase retrieval, we obtained an image of the paint sample that shows the distribution of the pigment particles and is consistent with the result obtained from a transmission x-ray microscope. The technique has been experimentally proven to be a feasible coherent x-ray imaging method with about 120 nm spatial resolution and was shown to work well with industrially relevant specimens.

  6. Diffraction crystals for sagittally focusing x-rays

    DOE Patents [OSTI]

    Ice, G.E.; Sparks, C.J. Jr.

    1982-06-07

    The invention is a new type of diffraction crystal designed for sagittally focusing photons of various energies. The invention is based on the discovery that such focusing is not obtainable with conventional crystals because of distortion resulting from anticlastic curvature. The new crystal comprises a monocrystalline base having a front face contoured for sagittally focusing photons and a back face provided with rigid, upstanding, stiffening ribs restricting anticlastic curvature. When mounted in a suitable bending device, the reflecting face of the crystal can be adjusted to focus photons having any one of a range of energies.

  7. Diffraction crystal for sagittally focusing x-rays

    DOE Patents [OSTI]

    Ice, Gene E.; Sparks, Jr., Cullie J.

    1984-01-01

    The invention is a new type of diffraction crystal designed for sagittally focusing photons of various energies. The invention is based on the discovery that such focusing is not obtainable with conventional crystals because of distortion resulting from anticlastic curvature. The new crystal comprises a monocrystalline base having a front face contoured for sagittally focusing photons and a back face provided with rigid, upstanding, stiffening ribs restricting anticlastic curvature. When mounted in a suitable bending device, the reflecting face of the crystal can be adjusted to focus photons having any one of a range of energies.

  8. Crystallization and preliminary X-ray diffraction study of porcine carboxypeptidase B

    SciTech Connect (OSTI)

    Akparov, V. Kh.; Timofeev, V. I. Kuranova, I. P.

    2015-05-15

    Crystals of porcine pancreatic carboxypeptidase B have been grown in microgravity by the capillary counter-diffusion method through a gel layer. The X-ray diffraction study showed that the crystals belong to sp. gr. P4{sub 1}2{sub 1}2 and have the following unit-cell parameters: a = b = 79.58 Å, c = 100.51 Å; α = β = γ = 90.00°. The X-ray diffraction data set suitable for the determination of the three-dimensional structure at atomic resolution was collected from one of the grown crystals at the SPring 8 synchrotron facility to 0.98 Å resolution.

  9. In situ laser heating and radial synchrotron X-ray diffraction ina diamond anvil cell

    SciTech Connect (OSTI)

    Kunz, Martin; Caldwell, Wendel A.; Miyagi, Lowell; Wenk,Hans-Rudolf

    2007-06-29

    We report a first combination of diamond anvil cell radialx-ray diffraction with in situ laser heating. The laser-heating setup ofALS beamline 12.2.2 was modified to allow one-sided heating of a samplein a diamond anvil cell with an 80 W yttrium lithium fluoride laser whileprobing the sample with radial x-ray diffraction. The diamond anvil cellis placed with its compressional axis vertical, and perpendicular to thebeam. The laser beam is focused onto the sample from the top while thesample is probed with hard x-rays through an x-ray transparentboron-epoxy gasket. The temperature response of preferred orientation of(Fe,Mg)O is probed as a test experiment. Recrystallization was observedabove 1500 K, accompanied by a decrease in stress.

  10. Real-time Studies of Shocked Polycrystalline Materials with Single-Pulse X-ray Diffraction

    SciTech Connect (OSTI)

    Dane V. Morgan

    2011-05-25

    Characteristic K-α x-rays used for single-pulse XRD are conventionally produced by a 37-stage high-voltage Marx pulse generator coupled to a vacuum needle-and-washer x-ray diode via coaxial transmission line. A large field-of-view x-ray image plate detection system typically enables observation of several Debye-Scherrer rings. Recently, we have developed a fiber-optic reducer, coupled to a CCD camera, to obtain low-noise, large field-of-view images. The direct beam spot is produced by bremsstrahlung radiation attenuated by a twomillimeter tungsten beam stop. Determination of the direct beam position is necessary to perform the ring integration.

  11. High spatial resolution X-ray and gamma ray imaging system using diffraction crystals

    DOE Patents [OSTI]

    Smither, Robert K.

    2011-05-17

    A method and a device for high spatial resolution imaging of a plurality of sources of x-ray and gamma-ray radiation are provided. The device comprises a plurality of arrays, with each array comprising a plurality of elements comprising a first collimator, a diffracting crystal, a second collimator, and a detector.

  12. Use of X-ray diffraction to quantify amorphous supplementary cementitious materials in anhydrous and hydrated blended cements

    SciTech Connect (OSTI)

    Snellings, R.; Salze, A.; Scrivener, K.L.

    2014-10-15

    The content of individual amorphous supplementary cementitious materials (SCMs) in anhydrous and hydrated blended cements was quantified by the PONKCS [1] X-ray diffraction (XRD) method. The analytical precision and accuracy of the method were assessed through comparison to a series of mixes of known phase composition and of increasing complexity. A 2σ precision smaller than 2–3 wt.% and an accuracy better than 2 wt.% were achieved for SCMs in mixes with quartz, anhydrous Portland cement, and hydrated Portland cement. The extent of reaction of SCMs in hydrating binders measured by XRD was 1) internally consistent as confirmed through the standard addition method and 2) showed a linear correlation to the cumulative heat release as measured independently by isothermal conduction calorimetry. The advantages, limitations and applicability of the method are discussed with reference to existing methods that measure the degree of reaction of SCMs in blended cements.

  13. X-Ray Fluorescence (XRF) | Open Energy Information

    Open Energy Info (EERE)

    Dispersive Spectroscopy (WDS) typically performed using a SEM or EPMA, and X-Ray Diffraction (XRD) analyses. Rock Lab Analysis Core Analysis Cuttings Analysis Isotopic...

  14. A laboratory based system for Laue micro x-ray diffraction

    SciTech Connect (OSTI)

    Advanced Light Source; Tamura, Nobumichi; Lynch, P.A.; Stevenson, A.W.; Liang, D.; Parry, D.; Wilkins, S.; Tamura, N.

    2007-02-28

    A laboratory diffraction system capable of illuminating individual grains in a polycrystalline matrix is described. Using a microfocus x-ray source equipped with a tungsten anode and prefigured monocapillary optic, a micro-x-ray diffraction system with a 10 mum beam was developed. The beam profile generated by the ellipsoidal capillary was determined using the"knife edge" approach. Measurement of the capillary performance, indicated a beam divergence of 14 mrad and a useable energy bandpass from 5.5 to 19 keV. Utilizing the polychromatic nature of the incident x-ray beam and application of the Laue indexing software package X-Ray Micro-Diffraction Analysis Software, the orientation and deviatoric strain of single grains in a polycrystalline material can be studied. To highlight the system potential the grain orientation and strain distribution of individual grains in a polycrystalline magnesium alloy (Mg 0.2 wt percent Nd) was mapped before and after tensile loading. A basal (0002) orientation was identified in the as-rolled annealed alloy; after tensile loading some grains were observed to undergo an orientation change of 30 degrees with respect to (0002). The applied uniaxial load was measured as an increase in the deviatoric tensile strain parallel to the load axis (37 References).

  15. Cyclic olefin homopolymer-based microfluidics for protein crystallization and in situ X-ray diffraction

    SciTech Connect (OSTI)

    Emamzadah, Soheila [Department of Molecular Biology, University of Geneva, CH-1205 Geneva (Switzerland); Department of Biochemistry, University of Geneva, CH-1205 Geneva (Switzerland); Petty, Tom J. [Department of Molecular Biology, University of Geneva, CH-1205 Geneva (Switzerland); Biomedical Graduate Studies Genomics and Computational Biology Group, University of Pennsylvania, Philadelphia, PA 19104 (United States); De Almeida, Victor [Department of Molecular Biology, University of Geneva, CH-1205 Geneva (Switzerland); Department of Biochemistry, University of Geneva, CH-1205 Geneva (Switzerland); Nishimura, Taisuke [Department of Plant Biology, University of Geneva, CH-1205 Geneva (Switzerland); Joly, Jacques; Ferrer, Jean-Luc [Institut de Biologie Structurale J.-P. Ebel, CEA-CNRS-University J. Fourier, 38027 Grenoble CEDEX 1 (France); Halazonetis, Thanos D., E-mail: thanos.halazonetis@unige.ch [Department of Molecular Biology, University of Geneva, CH-1205 Geneva (Switzerland); Department of Biochemistry, University of Geneva, CH-1205 Geneva (Switzerland)

    2009-09-01

    A cyclic olefin homopolymer-based microfluidics system has been established for protein crystallization and in situ X-ray diffraction. Microfluidics is a promising technology for the rapid identification of protein crystallization conditions. However, most of the existing systems utilize silicone elastomers as the chip material which, despite its many benefits, is highly permeable to water vapour. This limits the time available for protein crystallization to less than a week. Here, the use of a cyclic olefin homopolymer-based microfluidics system for protein crystallization and in situ X-ray diffraction is described. Liquid handling in this system is performed in 2 mm thin transparent cards which contain 500 chambers, each with a volume of 320 nl. Microbatch, vapour-diffusion and free-interface diffusion protocols for protein crystallization were implemented and crystals were obtained of a number of proteins, including chicken lysozyme, bovine trypsin, a human p53 protein containing both the DNA-binding and oligomerization domains bound to DNA and a functionally important domain of Arabidopsis Morpheus molecule 1 (MOM1). The latter two polypeptides have not been crystallized previously. For X-ray diffraction analysis, either the cards were opened to allow mounting of the crystals on loops or the crystals were exposed to X-rays in situ. For lysozyme, an entire X-ray diffraction data set at 1.5 resolution was collected without removing the crystal from the card. Thus, cyclic olefin homopolymer-based microfluidics systems have the potential to further automate protein crystallization and structural genomics efforts.

  16. Transient x-ray diffraction with simultaneous imaging under high strain-rate loading

    SciTech Connect (OSTI)

    Fan, D.; E, J. C.; Zhao, F.; Luo, S. N.; Lu, L.; Li, B.; Qi, M. L.; Sun, T.; Fezzaa, K.; Chen, W.

    2014-11-15

    Real time, in situ, multiframe, diffraction, and imaging measurements on bulk samples under high and ultrahigh strain-rate loading are highly desirable for micro- and mesoscale sciences. We present an experimental demonstration of multiframe transient x-ray diffraction (TXD) along with simultaneous imaging under high strain-rate loading at the Advanced Photon Source beamline 32ID. The feasibility study utilizes high strain-rate Hopkinson bar loading on a Mg alloy. The exposure time in TXD is 2–3 μs, and the frame interval is 26.7–62.5 μs. Various dynamic deformation mechanisms are revealed by TXD, including lattice expansion or compression, crystal plasticity, grain or lattice rotation, and likely grain refinement, as well as considerable anisotropy in deformation. Dynamic strain fields are mapped via x-ray digital image correlation, and are consistent with the diffraction measurements and loading histories.

  17. Apparatus for X-ray diffraction microscopy and tomography of cryo specimens

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Beetz, T.; Howells, M. R.; Jacobsen, C.; Kao, C. -C.; Kirz, J.; Lima, E.; Mentes, T. O.; Miao, H.; Sanchez-Hanke, C.; Sayre, D.; et al

    2005-03-14

    An apparatus for diffraction microscopy of biological and materials science specimens is described. In this system, a coherent soft X-ray beam is selected with a pinhole, and the illuminated specimen is followed by an adjustable beamstop and CCD camera to record diffraction data from non-crystalline specimens. In addition, a Fresnel zone plate can be inserted to allow for direct imaging. The system makes use of a cryogenic specimen holder with cryotransfer capabilities to allow frozen hydrated specimens to be loaded. The specimen can be tilted over a range of ± 80 ° degrees for three-dimensional imaging; this is done bymore » computer-controlled motors, enabling automated alignment of the specimen through a tilt series. The system is now in use for experiments in soft X-ray diffraction microscopy.« less

  18. Analysis of surface integrity of grinded gears using Barkhausen noise analysis and x-ray diffraction

    SciTech Connect (OSTI)

    Vrkoslavov, Lucie; Louda, Petr; Malec, Ji?i

    2014-02-18

    The contribution is focused to present results of study grinded gears made of 18CrNiMo7-6 steel used in the wind power plant for support (service) purposes. These gears were case-hardened due to standard hard case and soft core formation. This heat treatment increases wear resistance and fatigue strength of machine parts. During serial production some troubles with surface integrity have occurred. When solving complex problems lots of samples were prepared. For grinding of gears were used different parameters of cutting speed, number of material removal and lots from different subsuppliers. Material characterization was carried out using Barkhausen noise analysis (BNA) device; X-ray diffraction (XRD) measurement of surface residual stresses was done as well. Depth profile of measured characteristics, e.g. magnetoelastic parameter and residual stress was obtained by step by step layers' removing using electrolytic etching. BNA software Viewscan was used to measure magnetizing frequency sweep (MFS) and magnetizing voltage sweep (MVS). Scanning of Magnetoelastic parameter (MP) endwise individual teeth were also carried out with Viewscan. These measurements were done to find problematic surface areas after grinding such as thermal damaged locations. Plots of the hardness and thickness of case-hardened layer on cross sections were measurered as well. Evaluation of structure of subsurface case-hardened layer and core was made on etched metallographic patterns. The aim of performed measurements was to find correlation between conditions of grinding, residual stresses and structural and magnetoelastic parameters. Based on correlation of measured values and technological parameters optimizing the production of gears will be done.

  19. Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

    SciTech Connect (OSTI)

    McGonegle, David Wark, Justin S.; Higginbotham, Andrew; Milathianaki, Despina; Remington, Bruce A.

    2015-08-14

    A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as may occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. The simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.

  20. Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Dao, E. Han; Sierra, Raymond G.; Laksmono, Hartawan; Lemke, Henrik T.; Alonso-Mori, Roberto; Coey, Aaron; Larsen, Kevin; Baxter, Elizabeth L.; Cohen, Aina E.; Soltis, S. Michael; et al

    2015-04-30

    In this work, we collected radiation-damage-free data from a set of cryo-cooled crystals for a novel 30S ribosomal subunit mutant using goniometer-based femtosecond crystallography. Crystal quality assessment for these samples was conducted at the X-ray Pump Probe end-station of the Linac Coherent Light Source (LCLS) using recently introduced goniometer-based instrumentation. These 30S subunit crystals were genetically engineered to omit a 26-residue protein, Thx, which is present in the wild-type Thermus thermophilus 30S ribosomal subunit. We are primarily interested in elucidating the contribution of this ribosomal protein to the overall 30S subunit structure. To assess the viability of this study, femtosecondmore » X-ray diffraction patterns from these crystals were recorded at the LCLS during a protein crystal screening beam time. During our data collection, we successfully observed diffraction from these difficult-to-grow 30S ribosomal subunit crystals. Most of our crystals were found to diffract to low resolution, while one crystal diffracted to 3.2 Å resolution. These data suggest the feasibility of pursuing high-resolution data collection as well as the need to improve sample preparation and handling in order to collect a complete radiation-damage-free data set using an X-ray Free Electron Laser.« less

  1. Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

    SciTech Connect (OSTI)

    Dao, E. Han; Sierra, Raymond G.; Laksmono, Hartawan; Lemke, Henrik T.; Alonso-Mori, Roberto; Coey, Aaron; Larsen, Kevin; Baxter, Elizabeth L.; Cohen, Aina E.; Soltis, S. Michael; DeMirci, Hasan

    2015-04-30

    In this work, we collected radiation-damage-free data from a set of cryo-cooled crystals for a novel 30S ribosomal subunit mutant using goniometer-based femtosecond crystallography. Crystal quality assessment for these samples was conducted at the X-ray Pump Probe end-station of the Linac Coherent Light Source (LCLS) using recently introduced goniometer-based instrumentation. These 30S subunit crystals were genetically engineered to omit a 26-residue protein, Thx, which is present in the wild-type Thermus thermophilus 30S ribosomal subunit. We are primarily interested in elucidating the contribution of this ribosomal protein to the overall 30S subunit structure. To assess the viability of this study, femtosecond X-ray diffraction patterns from these crystals were recorded at the LCLS during a protein crystal screening beam time. During our data collection, we successfully observed diffraction from these difficult-to-grow 30S ribosomal subunit crystals. Most of our crystals were found to diffract to low resolution, while one crystal diffracted to 3.2 Å resolution. These data suggest the feasibility of pursuing high-resolution data collection as well as the need to improve sample preparation and handling in order to collect a complete radiation-damage-free data set using an X-ray Free Electron Laser.

  2. Method for characterizing mask defects using image reconstruction from X-ray diffraction patterns

    DOE Patents [OSTI]

    Hau-Riege, Stefan Peter

    2007-05-01

    The invention applies techniques for image reconstruction from X-ray diffraction patterns on the three-dimensional imaging of defects in EUVL multilayer films. The reconstructed image gives information about the out-of-plane position and the diffraction strength of the defect. The positional information can be used to select the correct defect repair technique. This invention enables the fabrication of defect-free (since repaired) X-ray Mo--Si multilayer mirrors. Repairing Mo--Si multilayer-film defects on mask blanks is a key for the commercial success of EUVL. It is known that particles are added to the Mo--Si multilayer film during the fabrication process. There is a large effort to reduce this contamination, but results are not sufficient, and defects continue to be a major mask yield limiter. All suggested repair strategies need to know the out-of-plane position of the defects in the multilayer.

  3. Induced magnetic anisotropy in Si-free nanocrystalline soft magnetic materials: A transmission x-ray diffraction study

    SciTech Connect (OSTI)

    Parsons, R. Suzuki, K.; Yanai, T.; Kishimoto, H.; Kato, A.; Ohnuma, M.

    2015-05-07

    In order to better understand the origin of field-induced anisotropy (K{sub u}) in Si-free nanocrystalline soft magnetic alloys, the lattice spacing of the bcc-Fe phase in nanocrystalline Fe{sub 94?x}Nb{sub 6}B{sub x} (x?=?10, 12, 14) alloys annealed under an applied magnetic field has been investigated by X-ray diffraction in transmission geometry (t-XRD) with the diffraction vector parallel and perpendicular to the field direction. The saturation magnetostriction (?{sub s}) of nanocrystalline Fe{sub 94?x}Nb{sub 6}B{sub x} was found to increase linearly with the volume fraction of the residual amorphous phase and is well described by taking into account the volume-weighted average of two local ?{sub s} values for the bcc-Fe nanocrystallites (?5??2?ppm) and the residual amorphous matrix (+8??2?ppm). The lattice distortion required to produce the measured K{sub u} values (?100?J/m{sup 3}) was estimated via the inverse magnetostrictive effect using the measured ?{sub s} values and was compared to the lattice spacing estimations made by t-XRD. The lattice strain required to produce K{sub u} under the magnetoelastic model was not observed by the t-XRD experiments and so the findings of this study suggest that the origin of magnetic field induced K{sub u} cannot be explained through the magnetoelastic effect.

  4. Azine bridged silver coordination polymers: Powder X-ray diffraction route to crystal structure determination of silver benzotriazole

    SciTech Connect (OSTI)

    Rajeswaran, Manju . E-mail: manju.rajeswaran@kodak.com; Blanton, Thomas N.; Giesen, David J.; Whitcomb, David R.; Zumbulyadis, Nicholas; Antalek, Brian J.; Neumann, Marcus M.; Misture, Scott T.

    2006-04-15

    In continuation of our interest in solid-state structures of silver complexes of photographic importance, the structure for silver benzotriazole (AgBZT), has now been obtained. The preferred method for solving crystal structures is via single-crystal X-ray diffraction (XRD). However, for some materials, growing single crystals of appropriate size and quality is often difficult or even impossible. AgBZT is an example of such a silver complex with poor solubility. The usual routes to preparing single crystals using recrystallization from a cooperating solvent resulted in polycrystalline powder samples. We propose a crystal structure for AgBZT, solved from synchrotron X-ray powder diffraction data, using a direct-space Monte Carlo simulated annealing approach. AgBZT crystals are monoclinic (P2{sub 1} /c), with unit cell dimensions, a=14.8052(3) A, b=3.7498(4) A, c=12.3495(12) A, and {beta}=114.200(6){sup o}. The AgBZT complex is constructed from all three of the Benzotriazole (BZT) nitrogens bonding to a separate silver atom. As a consequence of this bonding mode, the structure is a highly cross-linked, coordination polymer.

  5. Elimination of higher-order diffraction using zigzag transmission grating in soft x-ray region

    SciTech Connect (OSTI)

    Zang, H. P.; Wang, C. K.; Gao, Y. L.; Zhou, W. M.; Kuang, L. Y.; Wei, L.; Fan, W.; Zhang, W. H.; Zhao, Z. Q.; Cao, L. F.; Gu, Y. Q.; Zhang, B. H.; Jiang, G.; Zhu, X. L.; Xie, C. Q.; Zhao, Y. D.; Cui, M. Q.

    2012-03-12

    We present a realization of the sinusoidal transmission function using a series of zigzag-profiled strips where the transmission takes on the binary values 0 and 1 in a two-dimensional distribution. A zigzag transmission grating of 1000 line/mm has been fabricated and demonstrated on the soft x-ray beam of synchrotron radiation. The axial single-order diffraction indicates that the zigzag transmission grating is adequate for spectroscopic application.

  6. Precise orientation of single crystals by a simple x-ray diffraction rocking curve method

    SciTech Connect (OSTI)

    Doucette, L.D.; Pereira da Cunha, M.; Lad, R.J.

    2005-03-01

    A simple method has been developed for accurately measuring the crystallographic orientation of a single crystal boule, employing a conventional four-circle x-ray diffraction arrangement in the rocking curve mode which relaxes the need for precise instrument and/or reference alignment. By acquiring a total of eight rocking curve measurements at specific orientations about the specimen azimuth, the absolute miscut angle between a crystal surface and the desired crystallographic plane can be resolved to within {+-}0.01 deg.

  7. Realizing in-plane surface diffraction by x-ray multiple-beam diffraction with large incidence angle

    SciTech Connect (OSTI)

    Huang, Xian-Rong Gog, Thomas; Assoufid, Lahsen; Peng, Ru-Wen; Siddons, D. P.

    2014-11-03

    Based on rigorous dynamical-theory calculations, we demonstrate the principle of an x-ray multiple-beam diffraction (MBD) scheme that overcomes the long-lasting difficulties of high-resolution in-plane diffraction from crystal surfaces. This scheme only utilizes symmetric reflection geometry with large incident angles but activates the out-of-plane and in-plane diffraction processes simultaneously and separately in the continuous MBD planes. The in-plane diffraction is realized by detoured MBD, where the intermediate diffracted waves propagate parallel to the surface, which corresponds to an absolute Bragg surface diffraction configuration that is extremely sensitive to surface structures. A series of MBD diffraction and imaging techniques may be developed from this principle to study surface/interface (misfit) strains, lateral nanostructures, and phase transitions of a wide range of (pseudo)cubic crystal structures, including ultrathin epitaxial films and multilayers, quantum dots, strain-engineered semiconductor or (multi)ferroic materials, etc.

  8. Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystals

    SciTech Connect (OSTI)

    Haugh, M. J. Jacoby, K. D.; Wu, M.; Loisel, G. P.

    2014-11-15

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

  9. Experimental developments to obtain real-time x-ray diffraction measurements in plate impact experiments

    SciTech Connect (OSTI)

    Gupta, Y.M.; Zimmerman, K.A.; Rigg, P.A.; Zaretsky, E.B.; Savage, D.M.; Bellamy, P.M.

    1999-10-01

    An experimental facility was developed to obtain real-time, quantitative, x-ray diffraction data in laboratory plate impact experiments. A powder gun, to generate plane wave loading in samples, was designed and built specifically to permit flash x-ray diffraction measurements in shock-compression experiments. Spatial resolution and quality of the diffracted signals were improved significantly over past attempts through partial collimation of the incident beam and the use of two-dimensional detectors to record data from shocked crystals. The experimental configuration and synchronization issues are discussed, and relevant details of the x-ray system and the powder gun are described. Representative results are presented from experiments designed to determine unit cell compression in shock-compressed LiF single crystals subjected to both elastic and elastic-plastic deformation, respectively. The developments described here are expected to be useful for examining lattice deformation and structural changes in shock wave compression studies. {copyright} {ital 1999 American Institute of Physics.}

  10. Time-resolved x-ray diffraction techniques for bulk polycrystalline materials under dynamic loading

    SciTech Connect (OSTI)

    Lambert, P. K.; Hustedt, C. J.; Zhao, M.; Ananiadis, A. G.; Hufnagel, T. C.; Vecchio, K. S.; Huskins, E. L.; Casem, D. T.; Gruner, S. M.; Tate, M. W.; Philipp, H. T.; Purohit, P.; Weiss, J. T.; Woll, A. R.; Kannan, V.; Ramesh, K. T.; Kenesei, P.; Okasinski, J. S.; Almer, J.

    2014-09-15

    We have developed two techniques for time-resolved x-ray diffraction from bulk polycrystalline materials during dynamic loading. In the first technique, we synchronize a fast detector with loading of samples at strain rates of ∼10{sup 3}–10{sup 4} s{sup −1} in a compression Kolsky bar (split Hopkinson pressure bar) apparatus to obtain in situ diffraction patterns with exposures as short as 70 ns. This approach employs moderate x-ray energies (10–20 keV) and is well suited to weakly absorbing materials such as magnesium alloys. The second technique is useful for more strongly absorbing materials, and uses high-energy x-rays (86 keV) and a fast shutter synchronized with the Kolsky bar to produce short (∼40 μs) pulses timed with the arrival of the strain pulse at the specimen, recording the diffraction pattern on a large-format amorphous silicon detector. For both techniques we present sample data demonstrating the ability of these techniques to characterize elastic strains and polycrystalline texture as a function of time during high-rate deformation.

  11. Multilayer graphene stacks grown by different methods-thickness measurements by X-ray diffraction, Raman spectroscopy and optical transmission

    SciTech Connect (OSTI)

    Tokarczyk, M. Kowalski, G.; Kępa, H.; Grodecki, K.; Drabińska, A.; Strupiński, W.

    2013-12-15

    X-ray diffraction, Raman spectroscopy and Optical absorption estimates of the thickness of graphene multi layer stacks (number of graphene layers) are presented for three different growth techniques. The objective of this work was focused on comparison and reconciliation of the two already widely used methods for thickness estimates (Raman and Absorption) with the calibration of the X-ray method as far as Scherer constant K is concerned and X-ray based Wagner-Aqua extrapolation method.

  12. X-ray third-order nonlinear dynamical diffraction in a crystal

    SciTech Connect (OSTI)

    Balyan, M. K.

    2015-12-15

    The dynamic diffraction of an X-ray wave in a crystal with a third-order nonlinear response to external field strength has been theoretically investigated. General equations for the wave propagation in crystal and nonlinear Takagi equations for both ideal and deformed crystals are derived. Integrals of motion are determined for the nonlinear problem of dynamic diffraction. The results of the numerical calculations of reflectivity in the symmetric Laue geometry for an incident plane wave and the intensity distributions on the output crystal surface for a point source are reported as an example.

  13. Real-time, high-resolution x-ray diffraction measurements on shocked crystals at a synchrotron facility

    SciTech Connect (OSTI)

    Gupta, Y. M.; Turneaure, Stefan J.; Perkins, K.; Zimmerman, K.; Arganbright, N.; Shen, G.; Chow, P.

    2012-12-15

    The Advanced Photon Source (APS) at Argonne National Laboratory was used to obtain real-time, high-resolution x-ray diffraction measurements to determine the microscopic response of shock-compressed single crystals. Disk shaped samples were subjected to plane shock wave compression by impacting them with half-inch diameter, flat-faced projectiles. The projectiles were accelerated to velocities ranging between 300 and 1200 m/s using a compact powder gun designed specifically for use at a synchrotron facility. The experiments were designed to keep the sample probed volume under uniaxial strain and constant stress for a duration longer than the 153.4 ns spacing between x-ray bunches. X-rays from a single pulse (<100 ps duration) out of the periodic x-ray pulses emitted by the synchrotron were used for the diffraction measurements. A synchronization and x-ray detection technique was developed to ensure that the measured signal was obtained unambiguously from the desired x-ray pulse incident on the sample while the sample was in a constant uniaxial strain state. The synchronization and x-ray detection techniques described can be used for a variety of x-ray measurements on shock compressed solids and liquids at the APS. Detailed procedures for applying the Bragg-Brentano parafocusing approach to single crystals at the APS are presented. Analytic developments to determine the effects of crystal substructure and non-ideal geometry on the diffraction pattern position and shape are presented. Representative real-time x-ray diffraction data, indicating shock-induced microstructural changes, are presented for a shock-compressed Al(111) sample. The experimental developments presented here provided, in part, the impetus for the Dynamic Compression Sector (DCS) currently under development at the APS. Both the synchronization/x-ray detection methods and the analysis equations for high-resolution single crystal x-ray diffraction can be used at the DCS.

  14. X-ray diffraction in the pulsed laser heated diamond anvil cell

    SciTech Connect (OSTI)

    Goncharov, Alexander F.; Struzhkin, Viktor V.; Dalton, D. Allen; Prakapenka, Vitali B.; Kantor, Innokenty; Rivers, Mark L.

    2010-11-15

    We have developed in situ x-ray synchrotron diffraction measurements of samples heated by a pulsed laser in the diamond anvil cell at pressure up to 60 GPa. We used an electronically modulated 2-10 kHz repetition rate, 1064-1075 nm fiber laser with 1-100 {mu}s pulse width synchronized with a gated x-ray detector (Pilatus) and time-resolved radiometric temperature measurements. This enables the time domain measurements as a function of temperature in a microsecond time scale (averaged over many events, typically more than 10 000). X-ray diffraction data, temperature measurements, and finite element calculations with realistic geometric and thermochemical parameters show that in the present experimental configuration, samples 4 {mu}m thick can be continuously temperature monitored (up to 3000 K in our experiments) with the same level of axial and radial temperature uniformities as with continuous heating. We find that this novel technique offers a new and convenient way of fine tuning the maximum sample temperature by changing the pulse width of the laser. This delicate control, which may also prevent chemical reactivity and diffusion, enables accurate measurement of melting curves, phase changes, and thermal equations of state.

  15. Automated high pressure cell for pressure jump x-ray diffraction

    SciTech Connect (OSTI)

    Brooks, Nicholas J.; Gauthe, Beatrice L. L. E.; Templer, Richard H.; Ces, Oscar; Seddon, John M.; Terrill, Nick J.; Rogers, Sarah E.

    2010-06-15

    A high pressure cell for small and wide-angle x-ray diffraction measurements of soft condensed matter samples has been developed, incorporating a fully automated pressure generating network. The system allows both static and pressure jump measurements in the range of 0.1-500 MPa. Pressure jumps can be performed as quickly as 5 ms, both with increasing and decreasing pressures. Pressure is generated by a motorized high pressure pump, and the system is controlled remotely via a graphical user interface to allow operation by a broad user base, many of whom may have little previous experience of high pressure technology. Samples are loaded through a dedicated port allowing the x-ray windows to remain in place throughout an experiment; this facilitates accurate subtraction of background scattering. The system has been designed specifically for use at beamline I22 at the Diamond Light Source, United Kingdom, and has been fully integrated with the I22 beamline control systems.

  16. Effect of H2O on the morphological changes of KNO3 formed on K2O/Al2O3 NOx storage materials: Fourier transform infra-red (FTIR) and time-resolved x-ray diffraction (TR-XRD) studies

    SciTech Connect (OSTI)

    Kim, Do Heui; Mudiyanselage, Kumudu K.; Szanyi, Janos; Hanson, Jonathan C.; Peden, Charles HF

    2014-02-27

    Based on combined FTIR and XRD studies, we report here that H2O induces a morphological change of KNO3 species formed on model K2O/Al2O3 NOx storage-reduction catalysts. Specifically as evidenced by FTIR, the contact of H2O with NO2 pre-adsorbed on K2O/Al2O3 promotes the transformation from bidentate (surface-like) KNO3 species to ionic (bulk-like) ones irrespective of K loadings. Once H2O is removed from the sample, a reversible transformation into bidentate KNO3 is observed, demonstrating a significant dependence of H2O on such morphological changes. TR-XRD results show the formation of two different types of bulk KNO3 phases (orthorhomobic and rhombohedral) in an as-impregnated sample. Once H2O begins to desorb above 400 K, the former is transformed into the latter, resulting in the existence of only the rhombohedral KNO3 phase. On the basis of consistent FTIR and TR-XRD results, we propose a model for the morphological changes of KNO3 species with respect to NO2 adsorption/desorption, H2O and/or heat treatments. Compared with the BaO/Al2O3 system, K2O/Al2O3 shows some similarities with respect to the formation of bulk nitrates upon H2O contact. However, there are significant differences that originate from the lower melting temperature of KNO3 relative to Ba(NO3)2.

  17. X-ray diffraction study of short-period AlN/GaN superlattices

    SciTech Connect (OSTI)

    Kyutt, R. N. Shcheglov, M. P.; Ratnikov, V. V.; Yagovkina, M. A.; Davydov, V. Yu.; Smirnov, A. N.; Rozhavskaya, M. M.; Zavarin, E. E.; Lundin, V. V.

    2013-12-15

    The structure of short-period hexagonal GaN/AlN superlattices (SLs) has been investigated by X-ray diffraction. The samples have been grown by metalorganic vapor-phase epitaxy (MOVPE) in a horizontal reactor at a temperature of 1050°C on (0001)Al{sub 2}O{sub 3} substrates using GaN and AlN buffer layers. The SL period changes from 2 to 6 nm, and the thickness of the structure varies in a range from 0.3 to 1 μm. The complex of X-ray diffraction techniques includes a measurement of θ-2θ rocking curves of symmetric Bragg reflection, the construction of intensity maps for asymmetric reflections, a measurement and analysis of peak broadenings in different diffraction geometries, a precise measurement of lattice parameters, and the determination of radii of curvature. The thickness and strain of separate SL layers are determined by measuring the θ-2θ rocking curves subsequent simulation. It is shown that most SL samples are completely relaxed as a whole. At the same time, relaxation is absent between sublayers, which is why strains in the AlN and GaN sublayers (on the order of 1.2 × 10{sup −2}) have different signs. An analysis of diffraction peak half-widths allows us to determine the densities of individual sets of dislocations and observe their change from buffer layers to SLs.

  18. X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Zhou, X. Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A.; Yefanov, Oleksandr; Han, Gye Won; et al

    2016-04-12

    Here, serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solvedmore » with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.« less

  19. Data preparation and evaluation techniques for x-ray diffraction microscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Steinbrener, Jan; Nelson, Johanna; Huang, Xiaojing; Marchesini, Stefano; Shapiro, David; Turner, Joshua J.; Jacobsen, Chris

    2010-01-01

    The post-experiment processing of X-ray Diffraction Microscopy data is often time-consuming and difficult. This is mostly due to the fact that even if a preliminary result has been reconstructed, there is no definitive answer as to whether or not a better result with more consistently retrieved phases can still be obtained. In addition, we show here that the first step in data analysis, the assembly of two-dimensional diffraction patterns from a large set of raw diffraction data, is crucial to obtaining reconstructions of highest possible consistency. We have developed software that automates this process and results in consistently accurate diffractionmore » patterns. We have furthermore derived some criteria of validity for a tool commonly used to assess the consistency of reconstructions, the phase retrieval transfer function, and suggest a modified version that has improved utility for judging reconstruction quality.« less

  20. Fixture for supporting and aligning a sample to be analyzed in an x-ray diffraction apparatus

    DOE Patents [OSTI]

    Green, L.A.; Heck, J.L. Jr.

    1985-04-23

    A fixture is provided for supporting and aligning small samples of material on a goniometer for x-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the x-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an x-ray diffraction apparatus previously limited to the analysis of much larger samples.

  1. Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

    DOE Patents [OSTI]

    Green, Lanny A.; Heck, Jr., Joaquim L.

    1987-01-01

    A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

  2. High resolution x-ray and gamma ray imaging using diffraction lenses with mechanically bent crystals

    DOE Patents [OSTI]

    Smither, Robert K.

    2008-12-23

    A method for high spatial resolution imaging of a plurality of sources of x-ray and gamma-ray radiation is provided. High quality mechanically bent diffracting crystals of 0.1 mm radial width are used for focusing the radiation and directing the radiation to an array of detectors which is used for analyzing their addition to collect data as to the location of the source of radiation. A computer is used for converting the data to an image. The invention also provides for the use of a multi-component high resolution detector array and for narrow source and detector apertures.

  3. Atomic motion of resonantly vibrating quartz crystal visualized by time-resolved X-ray diffraction

    SciTech Connect (OSTI)

    Aoyagi, Shinobu; Osawa, Hitoshi; Sugimoto, Kunihisa; Fujiwara, Akihiko

    2015-11-16

    Transient atomic displacements during a resonant thickness-shear vibration of AT-cut α-quartz are revealed by time-resolved X-ray diffraction under an alternating electric field. The lattice strain resonantly amplified by the alternating electric field is ∼10{sup 4} times larger than that induced by a static electric field. The resonantly amplified lattice strain is achieved by fast displacements of oxygen anions and collateral resilient deformation of Si−O−Si angles bridging rigid SiO{sub 4} tetrahedra, which efficiently transduce electric energy into elastic energy.

  4. Characteristics of a molybdenum X-pinch X-ray source as a probe source for X-ray diffraction studies

    SciTech Connect (OSTI)

    Zucchini, F.; Chauvin, C.; Combes, P.; Sol, D.; Loyen, A.; Roques, B.; Grunenwald, J.; Bland, S. N.

    2015-03-15

    X-ray emission from a molybdenum X-pinch has been investigated as a potential probe for the high pressure states made in dynamic compression experiments. Studies were performed on a novel 300 kA, 400 ns generator which coupled the load directly to a low inductance capacitor and switch combination. The X-pinch load consisted of 4 crossed molybdenum wires of 13 μm diameter, crossed at an angle of 62°. The load height was 10 mm. An initial x-ray burst generated at the wire crossing point, radiated in the soft x-ray range (hυ < 10 keV). This was followed, 2–5 ns later, by at least one harder x-ray burst (hυ > 10 keV) whose power ranged from 1 to 7 MW. Time integrated spectral measurements showed that the harder bursts were dominated by K-alpha emission; though, a lower level, wide band continuum up to at least 30 keV was also present. Initial tests demonstrated that the source was capable of driving Laue diffraction experiments, probing uncompressed samples of LiF and aluminium.

  5. Crystallization and preliminary X-ray diffraction study of phosphoribosyl pyrophosphate synthetase from E. Coli

    SciTech Connect (OSTI)

    Timofeev, V. I. Abramchik, Yu. A. Zhukhlistova, N. E. Kuranova, I. P.

    2015-09-15

    Enzymes of the phosphoribosyl pyrophosphate synthetase family (PRPPS, EC 2.7.6.1) catalyze the formation of 5-phosphoribosyl pyrophosphate (5-PRPP) from adenosine triphosphate and ribose 5-phosphate. 5-Phosphoribosyl pyrophosphate is an important intermediate in the synthesis of purine, pyrimidine, and pyridine nucleotides, as well as of the amino acids histidine and tryptophan. The crystallization conditions for E. coli PRPPS were found by the vapor-diffusion technique and were optimized to apply the capillary counter-diffusion technique. The X-ray diffraction data set was collected from the crystals grown by the counter-diffusion technique using a synchrotron radiation source to 3.1-Å resolution. The crystals of PRPPS belong to sp. gr. P6{sub 3}22 and have the following unit-cell parameters: a = b = 104.44 Å, c = 124.98 Å, α = β = 90°, γ = 120°. The collected X-ray diffraction data set is suitable for the solution of the three-dimensional structure of PRPPS at 3.1-Å resolution.

  6. Dynamic in-situ X-ray Diffraction of Catalyzed Alanates

    SciTech Connect (OSTI)

    Gross, K.J.; Sandrock, G.; Thomas, G.J.

    2000-11-01

    The discovery that hydrogen can be reversible absorbed and desorbed from NaAlH{sub 4} by the addition of catalysts has created an entirely new prospect for lightweight hydrogen storage. NaAlH{sub 4} releases hydrogen through the following set of decomposition reactions: NaAlH{sub 4} {r_arrow} 1/3({alpha}-Na{sub 3}AlH{sub 6}) + 2/3Al + H{sub 2} {r_arrow} NaH + Al + 3/2H{sub 2}. These decomposition reactions as well as the reverse recombination reactions were directly observed using time-resolved in-situ x-ray powder diffraction. These measurements were performed under conditions similar to those found in PEM fuel cell operations (hydrogen absorption: 50--70 C, 10--15 bar Hz, hydrogen resorption: 80--110 C, 5--100 mbar H{sub 2}). Catalyst doping was found to dramatically improve kinetics under these conditions. In this study, the alanate was doped with a catalyst by dry ball-milling NaAlH{sub 4} with 2 mol.% solid TiCl{sub 3}. X-ray diffraction clearly showed that TiCl{sub 3} reacts with NaAlH{sub 4} to form NaCl during the doping process. Partial desorption of NaAlH{sub 4} was even observed to occur during the catalyst doping process.

  7. Three-dimensional coherent X-ray diffractive imaging of whole frozen-hydrated cells

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Rodriguez, Jose A.; Xu, Rui; Chen, Chien -Chun; Huang, Zhifeng; Jiang, Huaidong; Chen, Allan L.; Raines, Kevin S.; Pryor, Jr., Alan; Nam, Daewoong; Wiegart, Lutz; et al

    2015-09-01

    Here, a structural understanding of whole cells in three dimensions at high spatial resolution remains a significant challenge and, in the case of X-rays, has been limited by radiation damage. By alleviating this limitation, cryogenic coherent diffractive imaging (cryo-CDI) can in principle be used to bridge the important resolution gap between optical and electron microscopy in bio-imaging. Here, the first experimental demonstration of cryo-CDI for quantitative three-dimensional imaging of whole frozen-hydrated cells using 8 Kev X-rays is reported. As a proof of principle, a tilt series of 72 diffraction patterns was collected from a frozen-hydrated Neospora caninum cell and themore » three-dimensional mass density of the cell was reconstructed and quantified based on its natural contrast. This three-dimensional reconstruction reveals the surface and internal morphology of the cell, including its complex polarized sub-cellular structure. Finally, it is believed that this work represents an experimental milestone towards routine quantitative three-dimensional imaging of whole cells in their natural state with spatial resolutions in the tens of nanometres.« less

  8. High-resolution diffraction microscopy using the plane-wave field of a nearly diffraction limited focused x-ray beam

    SciTech Connect (OSTI)

    Takahashi, Yukio; Nishino, Yoshinori; Ishikawa, Tetsuya; Tsutsumi, Ryosuke; Kubo, Hideto; Furukawa, Hayato; Mimura, Hidekazu; Matsuyama, Satoshi; Zettsu, Nobuyuki; Matsubara, Eiichiro; Yamauchi, Kazuto

    2009-08-01

    X-ray waves in the center of the beam waist of nearly diffraction limited focused x-ray beams can be considered to have amplitude and phase that are both almost uniform, i.e., they are x-ray plane waves. Here we report the results of an experimental demonstration of high-resolution diffraction microscopy using the x-ray plane wave of the synchrotron x-ray beam focused using Kirkpatrik-Baez mirrors. A silver nanocube with an edge length of {approx}100 nm is illuminated with the x-ray beam focused to a {approx}1 {mu}m spot at 12 keV. A high-contrast symmetric diffraction pattern of the nanocube is observed in the forward far field. An image of the nanocube is successfully reconstructed by an iterative phasing method and its half-period resolution is 3.0 nm. This method does not only dramatically improve the spatial resolution of x-ray microscopy but also is a key technology for realizing single-pulse diffractive imaging using x-ray free-electron lasers.

  9. Coherent X-ray diffraction imaging and characterization of strain in silicon-on-insulator nanostructures

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Xiong, Gang; Moutanabbir, Oussama; Reiche, Manfred; Harder, Ross; Robinson, Ian

    2014-12-06

    Coherent X-ray diffraction imaging (CDI) has emerged in the last decade as a promising high resolution lens-less imaging approach for the characterization of various samples. It has made significant technical progress through developments in source, algorithm and imaging methodologies thus enabling important scientific breakthroughs in a broad range of disciplines. In this report, we will introduce the principles of forward scattering CDI and Bragg geometry CDI (BCDI), with an emphasis on the latter. BCDI exploits the ultra-high sensitivity of the diffraction pattern to the distortions of crystalline lattice. Its ability of imaging strain on the nanometer scale in three dimensionsmore » is highly novel. We will present the latest progress on the application of BCDI in investigating the strain relaxation behavior in nanoscale patterned strained silicon-on-insulator (sSOI) materials, aiming to understand and engineer strain for the design and implementation of new generation semiconductor devices.« less

  10. Coherent X-ray diffraction imaging and characterization of strain in silicon-on-insulator nanostructures

    SciTech Connect (OSTI)

    Xiong, Gang; Moutanabbir, Oussama; Reiche, Manfred; Harder, Ross; Robinson, Ian

    2014-12-06

    Coherent X-ray diffraction imaging (CDI) has emerged in the last decade as a promising high resolution lens-less imaging approach for the characterization of various samples. It has made significant technical progress through developments in source, algorithm and imaging methodologies thus enabling important scientific breakthroughs in a broad range of disciplines. In this report, we will introduce the principles of forward scattering CDI and Bragg geometry CDI (BCDI), with an emphasis on the latter. BCDI exploits the ultra-high sensitivity of the diffraction pattern to the distortions of crystalline lattice. Its ability of imaging strain on the nanometer scale in three dimensions is highly novel. We will present the latest progress on the application of BCDI in investigating the strain relaxation behavior in nanoscale patterned strained silicon-on-insulator (sSOI) materials, aiming to understand and engineer strain for the design and implementation of new generation semiconductor devices.

  11. X-ray and neutron diffraction of Er-hydride films.

    SciTech Connect (OSTI)

    Rodriguez, Mark Andrew

    2004-10-01

    The outline of this report is: (1) structures of hexagonal Er meal, ErH{sub 2} fluorite, and molybdenum; (2) texture issues and processing effects; (3) idea of pole figure integration; and (4) promising neutron diffraction work. Summary of this report are: (1) ErD{sub 2} and ErT{sub 2} film microstructures are strongly effected by processing conditions; (2) both x-ray and neutron diffraction are being pursued to help diagnose structure/property issues regarding ErT{sub 2} films and these correlations to He retention/release; (3) texture issues are great challenges for determination of site occupancy; and (4) work on pole-figure-integration looks to have promise addressing texture issues in ErD{sub 2} and ErT{sub 2} films.

  12. High-pressure X-ray diffraction and X-ray emission studies on iron-bearing silicate perovskite under high pressures

    SciTech Connect (OSTI)

    Lin, Jung-Fu; Speciale, Sergio; Prakapenka, Vitali B.; Dera, Przemek; Lavina, Babara; Watson, Heather C.

    2010-06-22

    Iron-bearing silicate perovskite is believed to be the most abundant mineral of the Earth's lower mantle. Recent studies have shown that Fe{sup 2+} exists predominantly in the intermediate-spin state with a total spin number of 1 in silicate perovskite in the lower part of the lower mantle. Here we have measured the spin states of iron and the pressure-volume relation in silicate perovskite [(Mg{sub 0.6},Fe{sub 0.4})SiO{sub 3}] at pressure conditions relevant to the lowermost mantle using in situ X-ray emission and X-ray diffraction in a diamond cell. Our results showed that the intermediate-spin Fe{sup 2+} is stable in the silicate perovskite up to {approx} 125 GPa but starts to transition to the low-spin state at approximately 135 GPa. Concurrent X-ray diffraction measurements showed a decrease of approximately 1% in the unit cell volume in the silicate perovskite [(Mg{sub 0.6},Fe{sub 0.4})SiO{sub 3}], which is attributed to the intermediate-spin to the low-spin transition. The transition pressure coincides with the pressure conditions of the lowermost mantle, raising the possibility of the existence of the silicate perovskite phase with the low-spin Fe{sup 2+} across the transition from the post-perovskite to the perovskite phases in the bottom of the D{double_prime} layer.

  13. A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

    SciTech Connect (OSTI)

    Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

    2015-08-11

    Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 l) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (1015 m) loaded into the chips yielded a complete, high-resolution (<1.6 ) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.

  14. A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

    2015-08-11

    Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

  15. Hand-held X-Ray Fluorescence (XRF) | Open Energy Information

    Open Energy Info (EERE)

    Dispersive Spectroscopy (WDS) typically performed using a SEM or EPMA, and X-Ray Diffraction (XRD) analyses. Data Collection and Mapping 2-M Probe Survey Fault Mapping Field...

  16. X-Ray Diffraction (XRD) At Long Valley Caldera Geothermal Area...

    Open Energy Info (EERE)

    studies, and seem to prove useful in most cases (Flexser, 1991; Goff et al., 1991; Smith and Suemnicht, 1991). Results from these studies are also summarized in Sorey et al....

  17. An experimental system for high temperature X-ray diffraction studies with in situ mechanical loading

    SciTech Connect (OSTI)

    Oswald, Benjamin B.; Pagan, Darren C.; Miller, Matthew P.; Schuren, Jay C.

    2013-03-15

    An experimental system with in situ thermomechanical loading has been developed to enable high energy synchrotron x-ray diffraction studies of crystalline materials. The system applies and maintains loads of up to 2250 N in uniaxial tension or compression at a frequency of up to 100 Hz. The furnace heats the specimen uniformly up to a maximum temperature of 1200 Degree-Sign C in a variety of atmospheres (oxidizing, inert, reducing) that, combined with in situ mechanical loading, can be used to mimic processing and operating conditions of engineering components. The loaded specimen is reoriented with respect to the incident beam of x-rays using two rotational axes to increase the number of crystal orientations interrogated. The system was used at the Cornell High Energy Synchrotron Source to conduct experiments on single crystal silicon and polycrystalline Low Solvus High Refractory nickel-based superalloy. The data from these experiments provide new insights into how stresses evolve at the crystal scale during thermomechanical loading and complement the development of high-fidelity material models.

  18. Multiple x-ray diffraction to determine transverse and longitudinal lattice deformation in shocked lithium fluoride

    SciTech Connect (OSTI)

    Rigg, P. A.; Gupta, Y. M.

    2001-03-01

    Experimental and analytic developments are described that utilize multiple x-ray diffraction to determine real-time, lattice deformation in directions parallel and perpendicular to shock-wave propagation in single crystals. Using a monochromatic x-ray source, two Bragg reflections were obtained simultaneously from LiF crystals shocked along the [111] and [100] directions. Symmetry permitted the transverse lattice deformation to be determined by measuring interplanar spacing longitudinally and in one other direction. We chose this to be a [110] direction in both cases because the intensity of the (220) reflection is high and because the transverse deformation component from this measurement is relatively large. Due to the complex geometry involved, an analytic model was required to calculate the (220) peak shift under the deformation conditions of interest. This model was used both to design experiments and to analyze the results. It was determined that shock compression below 4 GPa along the [111] orientation -- which results in macroscopic elastic deformation -- produced, as expected, no transverse lattice deformation. In contrast, shock compression along the [100] orientation -- which results in macroscopic elastic-plastic deformation -- produced equal interplanar spacing changes along the longitudinal and transverse directions. The analytic developments and the implications of our results are discussed.

  19. X-ray microstructural analysis of nanocrystalline TiZrN thin films by diffraction pattern modeling

    SciTech Connect (OSTI)

    Escobar, D.; Ospina, R.; Gmez, A.G.; Restrepo-Parra, E.; Arango, P.J.

    2014-02-15

    A detailed microstructural characterization of nanocrystalline TiZrN thin films grown at different substrate temperatures (T{sub S}) was carried out by X-ray diffraction (XRD). Total diffraction pattern modeling based on more meaningful microstructural parameters, such as crystallite size distribution and dislocation density, was performed to describe the microstructure of the thin films more precisely. This diffraction modeling has been implemented and used mostly to characterize powders, but the technique can be very useful to study hard thin films by taking certain considerations into account. Nanocrystalline films were grown by using the cathodic pulsed vacuum arc technique on stainless steel 316L substrates, varying the temperature from room temperature to 200 C. Further surface morphology analysis was performed to study the dependence of grain size on substrate temperature using atomic force microscopy (AFM). The crystallite and surface grain sizes obtained and the high density of dislocations observed indicate that the films underwent nanostructured growth. Variations in these microstructural parameters as a function of T{sub S} during deposition revealed a competition between adatom mobility and desorption processes, resulting in a specific microstructure. These films also showed slight anisotropy in their microstructure, and this was incorporated into the diffraction pattern modeling. The resulting model allowed for the films' microstructure during synthesis to be better understood according to the experimental results obtained. - Highlights: Mobility and desorption competition generates a critical temperature. A microstructure anisotropy related to the local strain was observed in thin films. Adatom mobility and desorption influence grain size and microstrain.

  20. An Improved X-ray Diffraction Method For Cellulose Crystallinity Measurement

    SciTech Connect (OSTI)

    Ju, Xiaohui; Bowden, Mark E.; Brown, Elvie E.; Zhang, Xiao

    2015-06-01

    We show in this work a modified X-ray diffraction method to determine cellulose crystallinity index (CrI). Nanocrystalline cellulose (NCC) dervided from bleached wood pulp was used as a model substrate. Rietveld refinement was applied with consideration of March-Dollase preferred orientation at the (001) plane. In contrast to most previous methods, three distinct amorphous peaks identified from new model samples which are used to calculate CrI. A 2 theta range from 10° to 75° was found to be more suitable to determine CrI and crystallite structural parameters such as d-spacing and crystallite size. This method enables a more reliable measurement of CrI of cellulose and may be applicable to other types of cellulose polymorphs.

  1. Structural Characterization of a Plutonium Sequestering Agent Complex by Synchrotron X-ray Diffraction

    SciTech Connect (OSTI)

    Gorden, A.E.V. |; Szigethy, G.; Tiedemann, B.E.F.; Xu, J.; Shuh, D.K.; Raymond, K.N. |

    2007-07-01

    New ligands and materials are required that can coordinate, sense, and purify actinides for selective extraction and reduction of toxic, radioactive wastes from the mining and purification of actinides. The similarities in the chemical, biological transport, and distribution properties of Fe(III) and Pu(IV) inspired a bio-mimetic approach to the development of sequestering agents for actinides. A detailed evaluation of the structure and bonding of actinide coordinating ligands like these is important for the design of new selective ligand systems. Knowing the difficulty with working with the crystals resulting from these ligand systems and safe handling considerations for working with Pu, procedures were developed that utilize the Advanced Light Source of Lawrence Berkeley National Laboratory to determine the solid-state structures of Pu complexes by X-ray diffraction. (au0011tho.

  2. Quantification of thin film crystallographic orientation using X-ray diffraction with an area detector

    SciTech Connect (OSTI)

    Baker, Jessica L; Jimison, Leslie H; Mannsfeld, Stefan; Volkman, Steven; Yin, Shong; Subramanian, Vivek; Salleo, Alberto; Alivisatos, A Paul; Toney, Michael F

    2010-02-19

    As thin films become increasingly popular (for solar cells, LEDs, microelectronics, batteries), quantitative morphological information is needed to predict and optimize the film's electronic, optical and mechanical properties. This quantification can be obtained quickly and easily with X-ray diffraction using an area detector and synchrotron radiation in two simple geometries. In this paper, we describe a methodology for constructing complete pole figures for thin films with fiber texture (isotropic in-plane orientation). We demonstrate this technique on semicrystalline polymer films, self-assembled nanoparticle semiconductor films, and randomly-packed metallic nanoparticle films. This method can be immediately implemented to help understand the relationship between film processing and microstructure, enabling the development of better and less expensive electronic and optoelectronic devices.

  3. Kinetics of Methane Hydrate Decomposition Studied via in Situ Low Temperature X-ray Powder Diffraction

    SciTech Connect (OSTI)

    Everett, Susan M; Rawn, Claudia J; Keffer, David J.; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy Joe

    2013-01-01

    Gas hydrates are known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice termed self-preservation or anomalous preservation. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Two regions of slowed decomposition for methane hydrate, 180 200 K and 230 260 K, were observed, and the kinetics were studied by in situ low temperature x-ray powder diffraction. The kinetic constants for ice formation from methane hydrate were determined by the Avrami model within each region and activation energies, Ea, were determined by the Arrhenius plot. Ea determined from the data for 180 200 K was 42 kJ/mol and for 230 260 K was 22 kJ/mol. The higher Ea in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

  4. Developments in time-resolved high pressure x-ray diffraction using rapid compression and decompression

    SciTech Connect (OSTI)

    Smith, Jesse S.; Sinogeikin, Stanislav V.; Lin, Chuanlong; Rod, Eric; Bai, Ligang; Shen, Guoyin

    2015-07-15

    Complementary advances in high pressure research apparatus and techniques make it possible to carry out time-resolved high pressure research using what would customarily be considered static high pressure apparatus. This work specifically explores time-resolved high pressure x-ray diffraction with rapid compression and/or decompression of a sample in a diamond anvil cell. Key aspects of the synchrotron beamline and ancillary equipment are presented, including source considerations, rapid (de)compression apparatus, high frequency imaging detectors, and software suitable for processing large volumes of data. A number of examples are presented, including fast equation of state measurements, compression rate dependent synthesis of metastable states in silicon and germanium, and ultrahigh compression rates using a piezoelectric driven diamond anvil cell.

  5. X-ray diffraction of solid tin to 1.2 TPa

    SciTech Connect (OSTI)

    Lazicki, A.; Rygg, J. R.; Coppari, F.; Smith, R.; Fratanduono, D.; Kraus, R. G.; Collins, G. W.; Briggs, R.; Braun, D. G.; Swift, D. C.; Eggert, J. H.

    2015-08-12

    In this study, we report direct in situ measurements of the crystal structure of tin between 0.12 and 1.2 TPa, the highest stress at which a crystal structure has ever been observed. Using angle-dispersive powder x-ray diffraction, we find that dynamically compressed Sn transforms to the body-centered-cubic (bcc) structure previously identified by ambient-temperature quasistatic-compression studies and by zero-kelvin density-functional theory predictions between 0.06 and 0.16 TPa. However, we observe no evidence for the hexagonal close-packed (hcp) phase found by those studies to be stable above 0.16 TPa. Instead, our results are consistent with bcc up to 1.2 TPa. We conjecture that at high temperature bcc is stabilized relative to hcp due to differences in vibrational free energy.

  6. X-ray diffraction of solid tin to 1.2 TPa

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Lazicki, A.; Rygg, J. R.; Coppari, F.; Smith, R.; Fratanduono, D.; Kraus, R. G.; Collins, G. W.; Briggs, R.; Braun, D. G.; Swift, D. C.; et al

    2015-08-12

    In this study, we report direct in situ measurements of the crystal structure of tin between 0.12 and 1.2 TPa, the highest stress at which a crystal structure has ever been observed. Using angle-dispersive powder x-ray diffraction, we find that dynamically compressed Sn transforms to the body-centered-cubic (bcc) structure previously identified by ambient-temperature quasistatic-compression studies and by zero-kelvin density-functional theory predictions between 0.06 and 0.16 TPa. However, we observe no evidence for the hexagonal close-packed (hcp) phase found by those studies to be stable above 0.16 TPa. Instead, our results are consistent with bcc up to 1.2 TPa. We conjecturemore » that at high temperature bcc is stabilized relative to hcp due to differences in vibrational free energy.« less

  7. Purification, crystallization, and preliminary X-ray diffraction study of purine nucleoside phosphorylase from E. coli

    SciTech Connect (OSTI)

    Abramchik, Yu. A. Timofeev, V. I. Zhukhlistova, N. E.; Muravieva, T. I.; Esipov, R. S.; Kuranova, I. P.

    2015-07-15

    Crystals of E. coli purine nucleoside phosphorylase were grown in microgravity by the capillary counter-diffusion method through a gel layer. The X-ray diffraction data set suitable for the determination of the three-dimensional structure at atomic resolution was collected from one crystal at the Spring-8 synchrotron facility to 0.99 Å resolution. The crystals belong to sp. gr. P2{sub 1} and have the following unit-cell parameters: a = 74.1 Å, b = 110.2 Å, c = 88.2 Å, α = γ = 90°, β = 111.08°. The crystal contains six subunits of the enzyme comprising a hexamer per asymmetric unit. The hexamer is the biological active form of E. coli. purine nucleoside phosphorylase.

  8. A semianalytic model to extract differential linear scattering coefficients of breast tissue from energy dispersive x-ray diffraction measurements

    SciTech Connect (OSTI)

    LeClair, Robert J.; Boileau, Michel M.; Wang Yinkun [Department of Physics and Astronomy, Laurentian University, 935 Ramsey Lake Road, Sudbury, Ontario, P3E 2C6 (Canada) and Biomolecular Sciences Program, Laurentian University, 935 Ramsey Lake Road, Sudbury, Ontario, P3E 2C6 (Canada); Department of Physics and Astronomy, Laurentian University, 935 Ramsey Lake Road, Sudbury, Ontario, P3E 2C6 (Canada); Department of Physics and Astronomy, Laurentian University, 935 Ramsey Lake Road, Sudbury, Ontario, P3E 2C6 (Canada)

    2006-04-15

    The goal of this work is to develop a technique to measure the x-ray diffraction signals of breast biopsy specimens. A biomedical x-ray diffraction technology capable of measuring such signals may prove to be of diagnostic use to the medical field. Energy dispersive x-ray diffraction measurements coupled with a semianalytical model were used to extract the differential linear scattering coefficients [{mu}{sub s}(x)] of breast tissues on absolute scales. The coefficients describe the probabilities of scatter events occurring per unit length of tissue per unit solid angle of detection. They are a function of the momentum transfer argument, x=sin({theta}/2)/{lambda}, where {theta}=scatter angle and {lambda}=incident wavelength. The technique was validated by using a 3 mm diameter 50 kV polychromatic x-ray beam incident on a 5 mm diameter 5 mm thick sample of water. Water was used because good x-ray diffraction data are available in the literature. The scatter profiles from 6 deg. to 15 deg. in increments of 1 deg. were measured with a 3 mmx3 mmx2 mm thick cadmium zinc telluride detector. A 2 mm diameter Pb aperture was placed on top of the detector. The target to detector distance was 29 cm and the duration of each measurement was 10 min. Ensemble averages of the results compare well with the gold standard data of A. H. Narten [''X-ray diffraction data on liquid water in the temperature range 4 deg. C-200 deg. C, ORNL Report No. 4578 (1970)]. An average 7.68% difference for which most of the discrepancies can be attributed to the background noise at low angles was obtained. The preliminary measurements of breast tissue are also encouraging.

  9. Capture and X-ray diffraction studies of protein microcrystals in a microfluidic trap array

    SciTech Connect (OSTI)

    Lyubimov, Artem Y.; Murray, Thomas D.; Koehl, Antoine; Araci, Ismail Emre; Uervirojnangkoorn, Monarin; Zeldin, Oliver B.; Cohen, Aina E.; Soltis, S. Michael; Baxter, Elizabeth L.; Brewster, Aaron S.; Sauter, Nicholas K.; Brunger, Axel T.; Berger, James M.

    2015-03-27

    X-ray free-electron lasers (XFELs) promise to enable the collection of interpretable diffraction data from samples that are refractory to data collection at synchrotron sources. At present, however, more efficient sample-delivery methods that minimize the consumption of microcrystalline material are needed to allow the application of XFEL sources to a wide range of challenging structural targets of biological importance. Here, a microfluidic chip is presented in which microcrystals can be captured at fixed, addressable points in a trap array from a small volume (<10 µl) of a pre-existing slurry grown off-chip. The device can be mounted on a standard goniostat for conducting diffraction experiments at room temperature without the need for flash-cooling. Proof-of-principle tests with a model system (hen egg-white lysozyme) demonstrated the high efficiency of the microfluidic approach for crystal harvesting, permitting the collection of sufficient data from only 265 single-crystal still images to permit determination and refinement of the structure of the protein. This work shows that microfluidic capture devices can be readily used to facilitate data collection from protein microcrystals grown in traditional laboratory formats, enabling analysis when cryopreservation is problematic or when only small numbers of crystals are available. Such microfluidic capture devices may also be useful for data collection at synchrotron sources.

  10. Capture and X-ray diffraction studies of protein microcrystals in a microfluidic trap array

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Lyubimov, Artem Y.; Murray, Thomas D.; Koehl, Antoine; Araci, Ismail Emre; Uervirojnangkoorn, Monarin; Zeldin, Oliver B.; Cohen, Aina E.; Soltis, S. Michael; Baxter, Elizabeth L.; Brewster, Aaron S.; et al

    2015-03-27

    X-ray free-electron lasers (XFELs) promise to enable the collection of interpretable diffraction data from samples that are refractory to data collection at synchrotron sources. At present, however, more efficient sample-delivery methods that minimize the consumption of microcrystalline material are needed to allow the application of XFEL sources to a wide range of challenging structural targets of biological importance. Here, a microfluidic chip is presented in which microcrystals can be captured at fixed, addressable points in a trap array from a small volume (<10 µl) of a pre-existing slurry grown off-chip. The device can be mounted on a standard goniostat formore » conducting diffraction experiments at room temperature without the need for flash-cooling. Proof-of-principle tests with a model system (hen egg-white lysozyme) demonstrated the high efficiency of the microfluidic approach for crystal harvesting, permitting the collection of sufficient data from only 265 single-crystal still images to permit determination and refinement of the structure of the protein. This work shows that microfluidic capture devices can be readily used to facilitate data collection from protein microcrystals grown in traditional laboratory formats, enabling analysis when cryopreservation is problematic or when only small numbers of crystals are available. Such microfluidic capture devices may also be useful for data collection at synchrotron sources.« less

  11. High-pressure behavior and thermoelastic properties of niobium studied by in situ x-ray diffraction

    SciTech Connect (OSTI)

    Zou, Yongtao E-mail: yongtaozou6@gmail.com; Li, Baosheng; Qi, Xintong; Wang, Xuebing; Chen, Ting; Li, Xuefei; Welch, David

    2014-07-07

    In situ synchrotron energy dispersive x-ray diffraction (XRD) experiments on Nb have been conducted at pressures up to 6.4 GPa and temperatures up to 1073 K. From the pressure-volume-temperature measurements, thermoelastic parameters were derived for the first time for Nb based on the thermal pressure (?P{sub th}) equation of state (EOS), modified high-T Birch-Murnaghan EOS, and Mie-Grneisen-Debye EOS. With the pressure derivative of the bulk modulus K{sub T}{sup } fixed at 4.0, we obtained the ambient isothermal bulk modulus K{sub T0}=174(5) GPa, the temperature derivative of bulk modulus at constant pressure (?K{sub T}/?T){sub P}=-0.060(8) GPa K? and at constant volume (?K{sub T}/?T){sub V}=-0.046(8) GPa K?, the volumetric thermal expansivity ?{sub T}(T)=2.3(3)10??+0.3(2)10??T (K?), as well as the pressure dependence of thermal expansion (??/?P){sub T}=(?2.00.4)10?? K? GPa?. Fitting the present data to the Mie-Grneisen-Debye EOS with Debye temperature ??=276.6 K gives ??=1.27(8) and K{sub T0}=171(3) GPa at a fixed value of q=3.0. The ambient isothermal bulk modulus and Grneisen parameter derived from this work are comparable to previously reported values from both experimental and theoretical studies. An in situ high-resolution, angle dispersive XRD study on Nb did not indicate any anomalous behavior related to pressure-induced electronic topological transitions at ~5 GPa as has been reported previously.

  12. Real-time observation of coherent acoustic phonons generated by an acoustically mismatched optoacoustic transducer using x-ray diffraction

    SciTech Connect (OSTI)

    Persson, A. I. H.; Andreasson, B. P.; Enquist, H.; Jurgilaitis, A.; Larsson, J.

    2015-11-14

    The spectrum of laser-generated acoustic phonons in indium antimonide coated with a thin nickel film has been studied using time-resolved x-ray diffraction. Strain pulses that can be considered to be built up from coherent phonons were generated in the nickel film by absorption of short laser pulses. Acoustic reflections at the Ni–InSb interface leads to interference that strongly modifies the resulting phonon spectrum. The study was performed with high momentum transfer resolution together with high time resolution. This was achieved by using a third-generation synchrotron radiation source that provided a high-brightness beam and an ultrafast x-ray streak camera to obtain a temporal resolution of 10 ps. We also carried out simulations, using commercial finite element software packages and on-line dynamic diffraction tools. Using these tools, it is possible to calculate the time-resolved x-ray reflectivity from these complicated strain shapes. The acoustic pulses have a peak strain amplitude close to 1%, and we investigated the possibility to use this device as an x-ray switch. At a bright source optimized for hard x-ray generation, the low reflectivity may be an acceptable trade-off to obtain a pulse duration that is more than an order of magnitude shorter.

  13. Boron phosphide under pressure: In situ study by Raman scattering and X-ray diffraction

    SciTech Connect (OSTI)

    Solozhenko, Vladimir L.; Kurakevych, Oleksandr O.; Le Godec, Yann; Kurnosov, Aleksandr V.; Oganov, Artem R.

    2014-07-21

    Cubic boron phosphide, BP, has been studied in situ by X-ray diffraction and Raman scattering up to 55?GPa at 300?K in a diamond anvil cell. The bulk modulus of B{sub 0}?=?174(2) GPa has been established, which is in excellent agreement with our ab initio calculations. The data on Raman shift as a function of pressure, combined with equation-of-state (EOS) data, allowed us to estimate the Grneisen parameters of the TO and LO modes of zinc-blende structure, ?{sub G}{sup TO?}=?1.26 and ?{sub G}{sup LO?}=?1.13, just like in the case of other A{sup III}B{sup V} diamond-like phases, for which ?{sub G}{sup TO?}>??{sub G}{sup LO?}??1. We also established that the pressure dependence of the effective electro-optical constant ? is responsible for a strong change in relative intensities of the TO and LO modes from I{sub TO}/I{sub LO}???0.25 at 0.1?MPa to I{sub TO}/I{sub LO}???2.5 at 45?GPa, for which we also find excellent agreement between experiment and theory.

  14. Pressure-temperature stability studies of FeOOH using x-ray diffraction

    SciTech Connect (OSTI)

    Gleason, Arianna E.; Jeanloz, Raymond; Kunz, Martin

    2008-07-21

    The Mie-Gruneisen formalism is used to fit a Birch-Murnaghan equation of state to high-temperature (T), high-pressure (P) X-ray diffraction unit-cell volume (V) measurements on synthetic goethite (alpha-FeOOH) to combined conditions of T = 23-250o C and P = 0-29.4 GPa. We find the zero-pressure thermal expansion coefficient of goethite to be alpha0 = 2.3 (+-0.6) x 10-5 K-1 over this temperature range. Our data yield zero-pressure compressional parameters: V0 = 138.75 (+- 0.02) Angstrom3, bulk modulus K0 = 140.3 (+- 3.7) GPa, pressure derivative K0' = 4.6 (+- 0.4), Gruneisen parameter gamma0 = 0.91 (+- 0.07), and Debye temperature Theta0 = 740 (+- 5) K. We identify decomposition conditions for 2alpha-FeOOH --> alpha-Fe2O3 + H2O at 1 - 8 GPa and 100-400oC, and the polymorphic transition from alpha-FeOOH (Pbnm) to epsilon-FeOOH (P21mn). The non-quenchable, high-pressure epsilon-FeOOH phase P-V data are fitted to a second-order (Birch) equation of state yielding, K0 = 158 (+- 5) GPa and V0 = 66.3 (+- 0.5) Angstrom3.

  15. An experimental apparatus for diffraction-limites soft x-ray nanofocusing

    SciTech Connect (OSTI)

    Merthe, Daniel; Goldberg, Kenneth; Yashchuk, Valeriy; Yuan, Sheng; McKinney, Wayne; Celestre, Richard; Mochi, Iacopo; Macdougall, James; Morrison, Gregory; Rakawa, Senajith; Anderson, Erik; Smith, Brian; Domning, Edward; Warwick, Tony; Padmore, Howard

    2011-10-21

    Realizing the experimental potential of high-brightness, next generation synchrotron and free-electron laser light sources requires the development of reflecting x-ray optics capable of wavefront preservation and high-resolution nano-focusing. At the Advanced Light Source (ALS) beamline 5.3.1, we are developing broadly applicable, high-accuracy, in situ, at-wavelength wavefront measurement techniques to surpass 100-nrad slope measurement accuracy for diffraction-limited Kirkpatrick-Baez (KB) mirrors. The at-wavelength methodology we are developing relies on a series of wavefront-sensing tests with increasing accuracy and sensitivity, including scanning-slit Hartmann tests, grating-based lateral shearing interferometry, and quantitative knife-edge testing. We describe the original experimental techniques and alignment methodology that have enabled us to optimally set a bendable KB mirror to achieve a focused, FWHM spot size of 150 nm, with 1 nm (1.24 keV) photons at 3.7 mrad numerical aperture. The predictions of wavefront measurement are confirmed by the knife-edge testing.The side-profiled elliptically bent mirror used in these one-dimensional focusing experiments was originally designed for a much different glancing angle and conjugate distances. This work demonstrates that high-accuracy, at-wavelength wavefront-slope feedback can be used to optimize the pitch, roll, and mirror-bending forces in situ, using procedures that are deterministic and repeatable.

  16. Deformation in metallic glasses studied by synchrotron x-ray diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Dmowski, Wojciech; Egami, Takeshi; Tong, Yang

    2016-01-11

    In this study, high mechanical strength is one of the superior properties of metallic glasses which render them promising as a structural material. However, understanding the process of mechanical deformation in strongly disordered matter, such as metallic glass, is exceedingly difficult because even an effort to describe the structure qualitatively is hampered by the absence of crystalline periodicity. In spite of such challenges, we demonstrate that high-energy synchrotron X-ray diffraction measurement under stress, using a two-dimensional detector coupled with the anisotropic pair-density function (PDF) analysis, has greatly facilitated the effort of unraveling complex atomic rearrangements involved in the elastic, anelastic,more » and plastic deformation of metallic glasses. Even though PDF only provides information on the correlation between two atoms and not on many-body correlations, which are often necessary in elucidating various properties, by using stress as means of exciting the system we can garner rich information on the nature of the atomic structure and local atomic rearrangements during deformation in glasses.« less

  17. Beyond crystallography: Diffractive imaging using coherent x-ray light sources

    SciTech Connect (OSTI)

    Miao, J.; Ishikawa, T.; Robinson, I. K.; Murnane, M. M.

    2015-04-30

    X-ray crystallography has been central to the development of many fields of science over the past century. It has now matured to a point that as long as good-quality crystals are available, their atomic structure can be routinely determined in three dimensions. However, many samples in physics, chemistry, materials science, nanoscience, geology, and biology are noncrystalline, and thus their three-dimensional structures are not accessible by traditional x-ray crystallography. Overcoming this hurdle has required the development of new coherent imaging methods to harness new coherent x-ray light sources. Here we review the revolutionary advances that are transforming x-ray sources and imaging in the 21st century.

  18. Microfluidic sorting of protein nanocrystals by size for X-ray free-electron laser diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Abdallah, Bahige G.; Zatsepin, Nadia A.; Roy-Chowdhury, Shatabdi; Coe, Jesse; Conrad, Chelsie E.; Dörner, Katerina; Sierra, Raymond G.; Stevenson, Hilary P.; Camacho-Alanis, Fernanda; Grant, Thomas D.; et al

    2015-08-19

    We report that the advent and application of the X-ray free-electron laser (XFEL) has uncovered the structures of proteins that could not previously be solved using traditional crystallography. While this new technology is powerful, optimization of the process is still needed to improve data quality and analysis efficiency. One area is sample heterogeneity, where variations in crystal size (among other factors) lead to the requirement of large data sets (and thus 10–100 mg of protein) for determining accurate structure factors. To decrease sample dispersity, we developed a high-throughput microfluidic sorter operating on the principle of dielectrophoresis, whereby polydisperse particles canmore » be transported into various fluid streams for size fractionation. Using this microsorter, we isolated several milliliters of photosystem I nanocrystal fractions ranging from 200 to 600 nm in size as characterized by dynamic light scattering, nanoparticle tracking, and electron microscopy. Sorted nanocrystals were delivered in a liquid jet via the gas dynamic virtual nozzle into the path of the XFEL at the Linac Coherent Light Source. We obtained diffraction to ~4 Å resolution, indicating that the small crystals were not damaged by the sorting process. We also observed the shape transforms of photosystem I nanocrystals, demonstrating that our device can optimize data collection for the shape transform-based phasing method. Using simulations, we show that narrow crystal size distributions can significantly improve merged data quality in serial crystallography. From this proof-of-concept work, we expect that the automated size-sorting of protein crystals will become an important step for sample production by reducing the amount of protein needed for a high quality final structure and the development of novel phasing methods that exploit inter-Bragg reflection intensities or use variations in beam intensity for radiation damage-induced phasing. Ultimately, this method

  19. X-ray Imaging Workshop

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    microscopy (PEEM), angle resolved photoemission spectroscopy (ARPES), coherent diffraction imaging, x-ray microscopy, micro-tomography, holographic imaging, and x-ray...

  20. Synchrotron X-ray powder diffraction and convergent beam electron diffraction studies on the cubic phase of MgV{sub 2}O{sub 4} spinel

    SciTech Connect (OSTI)

    Niitaka, Seiji; Lee, Soyeon; Oshima, Yoshifumi; Kato, Kenichi; Hashizume, Daisuke; Takata, Masaki; Takagi, Hidenori

    2014-07-01

    The A V{sub 2}O{sub 4} (A=Mg{sup 2+}, Zn{sup 2+}, Cd{sup 2+}) spinels are three-dimensional spin-1 frustrated systems with orbital degree of freedom, which have been known to possess intriguing orbital states causing releases of spin frustration at low temperatures. We have performed synchrotron X-ray and convergent beam electron diffraction measurements for one of these vanadates, MgV{sub 2}O{sub 4} in order to clarify its crystal structure in the high temperature cubic phase, which is regarded as an important starting point for understanding the details of the low temperature phase. We have successfully observed that the [001] zone axis convergent beam electron diffraction pattern exhibits 4mm symmetry, suggesting the space group of Fd3{sup ¯}m in the cubic MgV{sub 2}O{sub 4}. It has also been demonstrated that the crystal structure of the cubic MgV{sub 2}O{sub 4} contains VO{sub 6} octahedra elongated along the threefold rotation axis. Based on our results, we discuss the orbital states of MgV{sub 2}O{sub 4} as well as the other spinel vanadates. - Graphical abstract: Precise geometry of the VO{sub 6} octahedra in the cubic phase of MgV{sub 2}O{sub 4} spinel determined with the synchrotron powder XRD data. - Highlights: • We examined the crystal structure of the cubic phase of MgV{sub 2}O{sub 4} spinel. • We prepared the single crystal and powdered sample of MgV{sub 2}O{sub 4} with high quality. • The result of the CBED measurement agrees with the space group of Fd3{sup ¯}m in the phase. • The cubic phase has VO{sub 6} octahedra elongated along the threefold rotation axis.

  1. Structural hysteresis in dragline spider silks induced by supercontraction: an X-ray fiber micro-diffraction study

    SciTech Connect (OSTI)

    Sampath, Sujatha; Yarger, Jeffery L.

    2014-11-27

    Interaction with water causes shrinkage and significant changes in the structure of spider dragline silks, which has been referred to as supercontraction in the literature. Preferred orientation or alignment of protein chains with respect to the fiber axis is extensively changed during this supercontraction process. Synchrotron X-ray micro-fiber diffraction experiments have been performed on Nephila clavipes and Argiope aurantia major and minor ampullate dragline spider fibers in the native dry, contracted (by immersion in water) and restretched (from contracted) states. Changes in the orientation of β-sheet nanocrystallites and the oriented component of the amorphous network have been determined from wide-angle X-ray diffraction patterns. While both the crystalline and amorphous components lose preferred orientation on wetting with water, the nano-crystallites regain their orientation on wet-restretching, whereas the oriented amorphous components only partially regain their orientation. Dragline major ampullate silks in both the species contract more than their minor ampullate silks.

  2. Structural and chemical ordering of Heusler CoxMnyGez epitaxial films on Ge (111). Quantitative study using traditional and anomalous x-ray diffraction techniques

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Collins, B. A.; Chu, Y.; He, L.; Haskel, D.; Tsui, F.

    2015-12-14

    We found that epitaxial films of CoxMnyGez grown on Ge (111) substrates by molecular-beam-epitaxy techniques have been investigated as a continuous function of composition using combinatorial synchrotron x-ray diffraction (XRD) and x-ray fluorescence (XRF) spectroscopy techniques. A high-resolution ternary epitaxial phase diagram is obtained, revealing a small number of structural phases stabilized over large compositional regions. Ordering of the constituent elements in the compositional region near the full Heusler alloy Co2MnGe has been examined in detail using both traditional XRD and a new multiple-edge anomalous diffraction (MEAD) technique. Multiple-edge anomalous diffraction involves analyzing the energy dependence of multiple reflections acrossmore » each constituent absorption edge in order to detect and quantify the elemental distribution of occupation in specific lattice sites. Results of this paper show that structural and chemical ordering are very sensitive to the Co : Mn atomic ratio, such that the ordering is the highest at an atomic ratio of 2 but significantly reduced even a few percent off this ratio. The in-plane lattice is nearly coherent with that of the Ge substrate, while the approximately 2% lattice mismatch is accommodated by the out-of-plane tetragonal strain. Furthermore, the quantitative MEAD analysis reveals no detectable amount (<0.5%) of Co-Mn site swapping, but instead high levels (26%) of Mn-Ge site swapping. Increasing Ge concentration above the Heusler stoichiometry (Co 0.5 Mn 0.25 Ge 0.25 ) is shown to correlate with increased lattice vacancies, antisites, and stacking faults, but reduced lattice relaxation. The highest degree of chemical ordering is observed off the Heusler stoichiometry with a Ge enrichment of 5 at.%.« less

  3. Role of Molecular Structure on X-ray Diffraction in Thermotropic Uniaxial and Biaxial Nematic Liquid Crystal Phases

    SciTech Connect (OSTI)

    Acharya, Bharat R.; Kang, Shin-Woong; Prasad, Veena; Kumar, Satyendra

    2009-08-27

    X-ray diffraction is one of the most definitive methods to determine the structure of condensed matter phases, and it has been applied to unequivocally infer the structures of conventional calamitic and lyotropic liquid crystals. With the advent of bent-core and tetrapodic mesogens and the discovery of the biaxial nematic phase in them, the experimental results require more careful interpretation and analysis. Here, we present ab-initio calculations of X-ray diffraction patterns in the isotropic, uniaxial nematic, and biaxial nematic phases of bent-core mesogens. A simple Meier-Saupe-like molecular distribution function is employed to describe both aligned and unaligned mesophases. The distribution function is decomposed into two, polar and azimuthal, distribution functions to calculate the effect of the evolution of uniaxial and biaxial nematic orientational order. The calculations provide satisfactory semiquantitative interpretations of experimental results. The calculations presented here should provide a pathway to more refined and quantitative analysis of X-ray diffraction data from the biaxial nematic phase.

  4. Role of Molecular Structure on X-ray Diffraction in Uniaxial and Biaxial Phases of Thermotropic Liquid Crystals

    SciTech Connect (OSTI)

    Acharya, Bharat R.; Kang, Shin-Woong; Prasad, Veena; Kumar, Satyendra

    2009-04-29

    X-ray diffraction is one of the most definitive methods to determine the structure of condensed matter phases, and it has been applied to unequivocally infer the structures of conventional calamitic and lyotropic liquid crystals. With the advent of bent-core and tetrapodic mesogens and the discovery of the biaxial nematic phase in them, the experimental results require more careful interpretation and analysis. Here, we present ab-initio calculations of X-ray diffraction patterns in the isotropic, uniaxial nematic, and biaxial nematic phases of bent-core mesogens. A simple Meier-Saupe-like molecular distribution function is employed to describe both aligned and unaligned mesophases. The distribution function is decomposed into two, polar and azimuthal, distribution functions to calculate the effect of the evolution of uniaxial and biaxial nematic orientational order. The calculations provide satisfactory semiquantitative interpretations of experimental results. The calculations presented here should provide a pathway to more refined and quantitative analysis of X-ray diffraction data from the biaxial nematic phase.

  5. Simultaneous probing of phase transformations in Ni-Ti thin film shape memory alloy by synchrotron radiation-based X-ray diffraction and electrical resistivity

    SciTech Connect (OSTI)

    Braz Fernandes, F.M.; Silva, R.J.C.

    2013-02-15

    NickelTitanium (NiTi) thin film shape memory alloys (SMAs) have been widely projected as novel materials which can be utilized in microdevices. Characterization of their physical properties and its correlation with phase transformations has been a challenging issue. In the present study, X-ray beam diffraction has been utilized to obtain the structural information at different temperatures while cooling. Simultaneously, electrical resistivity (ER) was measured in the phase transformation temperature range. The variation of ER and integral area of the individual diffraction peaks of the different phases as a function of temperature have been compared. A mismatch between the conventional interpretation of ER variation and the results of the XRD data has been clearly identified. - Highlights: ? Phase transformation characterization of NiTi thin film SMA has been carried out. ? Simultaneous monitoring of the XRD and ER with temperature is performed. ? The variation of ER and integral area of the diffraction peaks have been compared. ? A shift of the transformation temperatures obtained by two techniques is discussed.

  6. X-ray diffraction study of the structure of detonation nanodiamonds

    SciTech Connect (OSTI)

    Ozerin, A. N. Kurkin, T. S.; Ozerina, L. A.; Dolmatov, V. Yu.

    2008-01-15

    The spatial structure of aggregates formed by detonation nanodiamonds is investigated using the wide-angle and small-angle X-ray scattering techniques. The effective sizes of crystallites and the crystallite size distribution function are determined. The shape of scattering aggregates is restored from the small-angle X-ray scattering data. An analysis of the results obtained allowed the conclusion that the nanodiamond aggregates have an extended spatial structure composed of nine to ten clusters, each involving four to five crystallites with a crystal lattice of the diamond type.

  7. A criterion for the dynamical to kinematical transition of x-ray diffraction on a bent crystal

    SciTech Connect (OSTI)

    Kushnir, V.I.; Macrander, A.T.

    1993-09-01

    It is well known that the peak reflectivity of a bent crystal, generally speaking, is smaller than that of a plane crystal, and it goes to zero when the crystal curvature goes to infinity. The reason for this is the transition between dynamical and kinematical diffraction that takes place as the crystal curvature increases. The physical explanation is as follows: the deviation from exact Bragg position along the beam changes so fast that the thickness over which the beam is within a Darwin width becomes too small to reflect the beam. Bent crystals are widely used as focusing elements in X-ray optics, and estimation of whether or not a bent crystal is still perfect enough to provide good reflectivity is of great importance. Currently the Advanced Photon Source (APS) is considering a number of bent crystals as focusing elements for future APS beamlines, including a sagittaly focusing monochromator and bent backscattering analyzer for inelastic X-ray scattering experiments. A criterion is given in answer to the question: To what extent is it possible to bend a crystal without loss of X-ray peak reflectivity? An expression based on the work of Chukhovskii, Gabrielyan and Petrashen, is formulated that applies to anisotropic cubic crystal and that can be used not only for conventional asymmetric Bragg diffraction, but also for inclined crystal diffraction. The following special cases are treated as examples: isotropic crystal, standard symmetrical Bragg diffraction, extremely asymmetric diffraction, and backscattering with Bragg angles near 90{degree}. In addition, an asymptotic behavior for high energies is detailed.

  8. X-ray diffraction, spectroscopic and DFT studies of 1-(4-bromophenyl)-3,5-diphenylformazan

    SciTech Connect (OSTI)

    Tezcan, H.; Tokay, N.; Alpaslan, G.; Erdnmez, A.

    2013-12-15

    The crystal structure of 1-(4-bromophenyl)-3,5-diphenylformazan was determined by X-ray single crystal diffraction technique. The crystals are orthorhombic, a = 23.0788(9), b = 7.9606(3), c = 18.6340(12) , Z = 8, sp. gr. Pbca, R{sub 1} = 0.074. The structure was also examined using the density-functional theory. Its structure stability, and frontier molecular orbital components were discussed and the results were compared with X-ray and spectral results. The maximum absorbtion peaks of the UV-vis spectrum of the compound have been calculated using the time-dependent density-functional theory. It was found a good agreement between the calculated and experimental maximum absorption wavelength.

  9. Quantitative analysis of the x-ray diffraction intensities of undulated smectic phases in bent-core liquid crystals

    SciTech Connect (OSTI)

    Folcia, C. L.; Etxebarria, J.; Ortega, J.

    2007-07-15

    X-ray diffraction diagrams of undulated smectic phases in bent-core liquid crystals have been theoretically studied. The intensities of the reflections have been obtained for different layer modulations, and a general expression has been deduced for orthogonal cells in terms of the different harmonics of the distortion. The case of sinusoidal modulation is especially simple and has been studied also in oblique cells. High-quality x-ray measurements of three compounds reported in the literature have been analyzed as examples. In all cases it has been deduced that the modulation is sinusoidal and its amplitude has been easily obtained by fitting the experimental intensities. Equatorial (h0) reflections have been also considered to obtain information about the structure of defects at the maxima and minima of the undulation.

  10. Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

    SciTech Connect (OSTI)

    Chagas, L.H.; De Carvalho, G.S.G.; San Gil, R.A.S.; Chiaro, S.S.X.; Leito, A.A.; Diniz, R.

    2014-01-01

    Graphical abstract: - Highlights: We synthesized three precursors of alumina from different methods. The calcination of the precursors generated several alumina polymorphs. XRD and NMR were used for structural investigation of the polymorphs. The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrational and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the ?-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.

  11. Purification, crystallization and preliminary X-ray diffraction analysis of the kinase domain of human tousled-like kinase 2

    SciTech Connect (OSTI)

    Garrote, Ana M.; Redondo, Pilar; Montoya, Guillermo; Muoz, Ins G.

    2014-02-19

    The C-terminal kinase domain of TLK2 (a human tousled-like kinase) has been cloned and overexpressed in Escherichia coli followed by purification to homogeneity. Crystallization experiments in the presence of ATP-?-S yielded crystals suitable for X-ray diffraction analysis belonging to two different space groups: tetragonal I4{sub 1}22 and cubic P2{sub 1}3. Tousled-like kinases (TLKs) are an evolutionarily conserved family of serine/threonine protein kinases involved in chromatin dynamics, including DNA replication and repair, transcription and chromosome segregation. The two members of the family reported in humans, namely TLK1 and TLK2, localize to the cell nucleus and are capable of forming homo- or hetero-oligomers by themselves. To characterize the role of TLK2, its C-terminal kinase domain was cloned and overexpressed in Escherichia coli followed by purification to homogeneity. Crystallization experiments in the presence of ATP-?-S yielded crystals suitable for X-ray diffraction analysis belonging to two different space groups: tetragonal I4{sub 1}22 and cubic P2{sub 1}3. The latter produced the best diffracting crystal (3.4 resolution using synchrotron radiation), with unit-cell parameters a = b = c = 126.05 , ? = ? = ? = 90. The asymmetric unit contained one protein molecule, with a Matthews coefficient of 4.59 {sup 3} Da{sup ?1} and a solvent content of 73.23%.

  12. 7 Resolution in Protein 2-Dimentional-Crystal X-Ray Diffraction at Linac Coherent Light Source

    SciTech Connect (OSTI)

    Pedrini, Bill; Tsai, Ching-Ju; Capitani, Guido; Padeste, Celestino; Hunter, Mark; Zatsepin, Nadia A.; Barty, Anton; Benner, Henry; Boutet, Sebastien; Feld, Geoffrey K.; Hau-Riege, Stefan; Kirian, Rick; Kupitz, Christopher; Messerschmidt, Marc; Ogren, John I.; Pardini, Tommaso; Segelke, Brent; Williams, Garth J.; Spence , John C.; Abela, Rafael; Coleman, Matthew A.; Evans, James E.; Schertler, Gebhard; Frank, Matthias; Li, Xiao-Dan

    2014-06-09

    Membrane proteins arranged as two-dimensional (2D) crystals in the lipid en- vironment provide close-to-physiological structural information, which is essential for understanding the molecular mechanisms of protein function. X-ray diffraction from individual 2D crystals did not represent a suitable investigation tool because of radiation damage. The recent availability of ultrashort pulses from X-ray Free Electron Lasers (X-FELs) has now provided a mean to outrun the damage. Here we report on measurements performed at the LCLS X-FEL on bacteriorhodopsin 2D crystals mounted on a solid support and kept at room temperature. By merg- ing data from about a dozen of single crystal diffraction images, we unambiguously identified the diffraction peaks to a resolution of 7 A, thus improving the observable resolution with respect to that achievable from a single pattern alone. This indicates that a larger dataset will allow for reliable quantification of peak intensities, and in turn a corresponding increase of resolution. The presented results pave the way to further X-FEL studies on 2D crystals, which may include pump-probe experiments at subpicosecond time resolution.

  13. Crystallization and preliminary X-ray diffraction analysis of the haem-binding protein HemS from Yersinia enterocolitica

    SciTech Connect (OSTI)

    Schneider, Sabine; Paoli, Massimo

    2005-08-01

    The haem binding protein HemS from Y. enterocolitica has been crystallized in complex with its ligand. The crystals diffracted X-rays to 2.6 Å in-house. Bacteria have evolved strategies to acquire iron from their environment. Pathogenic microbes rely on specialized proteins to ‘steal’ haem from their host and use it as an iron source. HemS is the ultimate recipient of a molecular-relay system for haem uptake in Gram-negative species, functioning as the cytosolic carrier of haem. Soluble expression and high-quality diffraction crystals were obtained for HemS from Yersinia enterocolitica. Crystals belong to the orthorhombic space group I222, with unit-cell parameters a = 74.86, b = 77.45, c = 114.09 Å, and diffract X-rays to 2.6 Å spacing in-house. Determination of the structure of the haem–HemS complex will reveal the molecular basis of haem binding.

  14. Simultaneous X-ray diffraction and phase-contrast imaging for investigating material deformation mechanisms during high-rate loading

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Hudspeth, M.; Sun, T.; Parab, N.; Guo, Z.; Fezzaa, K.; Luo, S.; Chen, W.

    2015-01-01

    Using a high-speed camera and an intensified charge-coupled device (ICCD), a simultaneous X-ray imaging and diffraction technique has been developed for studying dynamic material behaviors during high-rate tensile loading. A Kolsky tension bar has been used to pull samples at 1000 s–1and 5000 s–1strain-rates for super-elastic equiatomic NiTi and 1100-O series aluminium, respectively. By altering the ICCD gating time, temporal resolutions of 100 ps and 3.37 µs have been achieved in capturing the diffraction patterns of interest, thus equating to single-pulse and 22-pulse X-ray exposure. Furthermore, the sample through-thickness deformation process has been simultaneously imagedviaphase-contrast imaging. It is also shownmore » that adequate signal-to-noise ratios are achieved for the detected white-beam diffraction patterns, thereby allowing sufficient information to perform quantitative data analysis diffractionviain-house software (WBXRD_GUI). Finally, of current interest is the ability to evaluate crystald-spacing, texture evolution and material phase transitions, all of which will be established from experiments performed at the aforementioned elevated strain-rates.« less

  15. Texture, residual strain, and plastic deformation around scratches in alloy 600 using synchrotron x-ray Laue micro-diffraction.

    SciTech Connect (OSTI)

    Suominen Fuller, M. L.; Klassen, R. J.; McIntyre, N. S.; Gerson, A. R.; Ramamurthy, S.; King, P. J.; Liu, W.; Univ. of Western Ontario; Univ. of South Australia; Babcock & Wilcox Canada

    2008-01-01

    Deformation around two scratches in Alloy 600 (A600) was studied nondestructively using synchrotron Laue differential aperture X-ray microscopy. The orientation of grains and elastic strain distribution around the scratches were measured. A complex residual deviatoric elastic strain state was found to exist around the scratches. Heavy plastic deformation was observed up to a distance of 20 {micro}m from the scratches. In the region 20-30 {micro}m from the scratches the diffraction spots were heavily streaked and split indicating misoriented dislocation cell structures.

  16. X-ray nano-diffraction study of Sr intermetallic phase during solidification of Al-Si hypoeutectic alloy

    SciTech Connect (OSTI)

    Manickaraj, Jeyakumar; Gorny, Anton; Shankar, Sumanth, E-mail: shankar@mcmaster.ca [Light Metal Casting Research Centre (LMCRC), Department of Mechanical Engineering, McMaster University, 1280 Main Street W, Hamilton, Ontario L8S 4L7 (Canada); Cai, Zhonghou [Advanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States)

    2014-02-17

    The evolution of strontium (Sr) containing intermetallic phase in the eutectic reaction of Sr-modified Al-Si hypoeutectic alloy was studied with high energy synchrotron beam source for nano-diffraction experiments and x-ray fluorescence elemental mapping. Contrary to popular belief, Sr does not seem to interfere with the Twin Plane Re-entrant Edge (TPRE) growth mechanism of eutectic Si, but evolves as the Al{sub 2}Si{sub 2}Sr phase during the eutectic reaction at the boundary between the eutectic Si and Al grains.

  17. Sample cell for powder x-ray diffraction at up to 500 bars and 200 deg. C

    SciTech Connect (OSTI)

    Jupe, Andrew C.; Wilkinson, Angus P.

    2006-11-15

    A low cost sample cell for powder diffraction at high pressure and temperature that employs either sapphire or steel pressure tubes is described. The cell can be assembled rapidly, facilitating the study of chemically reacting systems, and it provides good control of both pressure and temperature in a regimen where diamond anvil cells and multianvil apparatus cannot be used. The design provides a relatively large sample volume making it suitable for the study of quite large grain size materials, such as hydrating cement slurries. However, relatively high energy x rays are needed to penetrate the pressure tube.

  18. Sample cell for powder x-ray diffraction at up to 500 bars and 200 °C

    SciTech Connect (OSTI)

    Jupe, Andrew C.; Wilkinson, Angus P.

    2008-10-03

    A low cost sample cell for powder diffraction at high pressure and temperature that employs either sapphire or steel pressure tubes is described. The cell can be assembled rapidly, facilitating the study of chemically reacting systems, and it provides good control of both pressure and temperature in a regimen where diamond anvil cells and multianvil apparatus cannot be used. The design provides a relatively large sample volume making it suitable for the study of quite large grain size materials, such as hydrating cement slurries. However, relatively high energy x rays are needed to penetrate the pressure tube.

  19. An assessment of the resolution limitation due to radiation-damage in X-ray diffraction microscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Howells, M. R.; Beetz, T.; Chapman, H. N.; Cui, C.; Holton, J. M.; Jacobsen, C. J.; Kirz, J.; Lima, E.; Marchesini, S.; Miao, H.; et al

    2008-11-17

    X-ray diffraction microscopy (XDM) is a new form of x-ray imaging that is being practiced at several third-generation synchrotron-radiation x-ray facilities. Nine years have elapsed since the technique was first introduced and it has made rapid progress in demonstrating high-resolution three-dimensional imaging and promises few-nm resolution with much larger samples than can be imaged in the transmission electron microscope. Both life- and materials-science applications of XDM are intended, and it is expected that the principal limitation to resolution will be radiation damage for life science and the coherent power of available x-ray sources for material science. In this paper wemore » address the question of the role of radiation damage. We use a statistical analysis based on the so-called "dose fractionation theorem" of Hegerl and Hoppe to calculate the dose needed to make an image of a single life-science sample by XDM with a given resolution. We find that for simply-shaped objects the needed dose scales with the inverse fourth power of the resolution and present experimental evidence to support this finding. To determine the maximum tolerable dose we have assembled a number of data taken from the literature plus some measurements of our own which cover ranges of resolution that are not well covered otherwise. The conclusion of this study is that, based on the natural contrast between protein and water and "Rose-criterion" image quality, one should be able to image a frozen-hydrated biological sample using XDM at a resolution of about 10 nm.« less

  20. X-ray diffraction study of Penicillium Vitale catalase in the complex with aminotriazole

    SciTech Connect (OSTI)

    Borovik, A. A.; Grebenko, A. I.; Melik-Adamyan, V. R.

    2011-07-15

    The three-dimensional structure of the enzyme catalase from Penicillium vitale in a complex with the inhibitor aminotriazole was solved and refined by protein X-ray crystallography methods. An analysis of the three-dimensional structure of the complex showed that the inhibition of the enzyme occurs as a result of the covalent binding of aminotriazole to the amino-acid residue His64 in the active site of the enzyme. An investigation of the three-dimensional structure of the complex resulted in the amino-acid residues being more precisely identified. The binding sites of saccharide residues and calcium ions in the protein molecule were found.

  1. Communication: X-ray coherent diffractive imaging by immersion in nanodroplets

    SciTech Connect (OSTI)

    Tanyag, Rico Mayro P.; Bernando, Charles; Jones, Curtis F.; Bacellar, Camila; Ferguson, Ken R.; Anielski, Denis; Boll, Rebecca; Carron, Sebastian; Cryan, James P.; Englert, Lars; Epp, Sascha W.; Erk, Benjamin; Foucar, Lutz; Gomez, Luis F.; Hartmann, Robert; Neumark, Daniel M.; Rolles, Daniel; Rudek, Benedikt; Rudenko, Artem; Siefermann, Katrin R.; Ullrich, Joachim; Weise, Fabian; Bostedt, Christoph; Gessner, Oliver; Vilesov, Andrey F.

    2015-10-14

    Lensless x-ray microscopy requires the recovery of the phase of the radiation scattered from a specimen. Here, we demonstrate a de novo phase retrieval technique by encapsulating an object in a superfluid helium nanodroplet, which provides both a physical support and an approximate scattering phase for the iterative image reconstruction. The technique is robust, fast-converging, and yields the complex density of the immersed object. As a result, images of xenon clusters embedded in superfluid helium droplets reveal transient configurations of quantum vortices in this fragile system.

  2. Communication: X-ray coherent diffractive imaging by immersion in nanodroplets

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Tanyag, Rico Mayro P.; Bernando, Charles; Jones, Curtis F.; Bacellar, Camila; Ferguson, Ken R.; Anielski, Denis; Boll, Rebecca; Carron, Sebastian; Cryan, James P.; Englert, Lars; et al

    2015-10-14

    Lensless x-ray microscopy requires the recovery of the phase of the radiation scattered from a specimen. Here, we demonstrate a de novo phase retrieval technique by encapsulating an object in a superfluid helium nanodroplet, which provides both a physical support and an approximate scattering phase for the iterative image reconstruction. The technique is robust, fast-converging, and yields the complex density of the immersed object. As a result, images of xenon clusters embedded in superfluid helium droplets reveal transient configurations of quantum vortices in this fragile system.

  3. Femtosecond diffractive imaging with a soft-X-ray free-electron laser (CXIDB ID 3)

    DOE Data Explorer [Office of Scientific and Technical Information (OSTI)]

    Chapman, H. N.

    2011-02-23

    The diffraction pattern of this entry corresponds to the one shown in **figure 2a** of the corresponding citation.

  4. Femtosecond diffractive imaging with a soft-X-ray free-electron laser (CXIDB ID 3)

    DOE Data Explorer [Office of Scientific and Technical Information (OSTI)]

    Chapman, H. N.

    The diffraction pattern of this entry corresponds to the one shown in **figure 2a** of the corresponding citation.

  5. High efficiency, high quality x-ray optic based on ellipsoidally bent highly oriented pyrolytic graphite crystal for ultrafast x-ray diffraction experiments

    SciTech Connect (OSTI)

    Uschmann, I.; Nothelle, U.; Foerster, E.; Arkadiev, V.; Langhoff, N.; Antonov, A.; Grigorieva, I.; Steinkopf, R.; Gebhardt, A

    2005-08-20

    By the use of a thin highly oriented pyrolytic graphite crystal (HOPG) bent to a high-performance ellipsoidal shape it was possible to focus monochromatic x-rays of 4.5 keV photon energy with an efficiency of 0.0033, which is 30 times larger than for previously used bent crystals. Isotropic TiK{sub a}lpha radiation of a 150 {mu}m source was focused onto a 450 {mu}m spot. The size of the focal spot can be explained by broadening due to the mosaic crystal rocking curve. The rocking curve width (FWHM) of the thin graphite foil was determined to 0.11 deg. . The estimated temporal broadening of an ultrashort Kalpha pulse by the crystal is not larger than 300 fs. These properties make the x-ray optic very attractive for ultrafast time-resolved x-ray measurements.

  6. X-ray diffraction study of the phase transformations in NiTi shape memory alloy

    SciTech Connect (OSTI)

    Uchil, J.; Fernandes, F.M. Braz . E-mail: kkmahesh@rediffmail.com

    2007-03-15

    The phase transformations occurring in heat-treated NiTi shape memory alloys have been studied through the analysis of variation in integrated peak area (integrated intensity) with temperature, under the XRD peak profiles in the transformation temperature range. For this purpose, integrated peak area under the prominent peak corresponding to (110) plane of the austenitic phase has been chosen. The results so obtained are compared with those got from the DSC method. The XRD method is found to be more sensitive.

  7. Mesoscopic structural phase progression in photo-excited VO2 revealed by time-resolved x-ray diffraction microscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Zhu, Yi; Cai, Zhonghou; Chen, Pice; Zhang, Qingteng; Highland, Matthew J.; Jung, II Woong; Walko, Donald A.; Dufresne, Eric M.; Jaewoo, Jeong; Samant, Mahesh G.; et al

    2016-02-26

    Dynamical phase separation during a solid-solid phase transition poses a challenge for understanding the fundamental processes in correlated materials. Critical information underlying a phase transition, such as localized phase competition, is difficult to reveal by measurements that are spatially averaged over many phase seperated regions. The ability to simultanousely track the spatial and temporal evolution of such systems is essential to understanding mesoscopic processes during a phase transition. Using state-of- the-art time-resolved hard x-ray diffraction microscopy, we directly visualize the structural phase progression in a VO2 film upon photoexcitation. Following a homogenous in-plane optical excitation, the phase transformation is initiatedmore » at discrete sites and completed by the growth of one lattice structure into the other, instead of a simultaneous isotropic lattice symmetry change. The time-dependent x-ray diffraction spatial maps show that the in-plane phase progression in laser-superheated VO2 is via a displacive lattice transformation as a result of relaxation from an excited monoclinic phase into a rutile phase. The speed of the phase front progression is quantitatively measured, which is faster than the process driven by in-plane thermal diffusion but slower than the sound speed in VO2. Lastly, the direct visualization of localized structural changes in the time domain opens a new avenue to study mesoscopic processes in driven systems.« less

  8. X-Ray Powder Diffraction Study of Synthetic Palmierite, K{sub 2}Pb(SO{sub 4}){sub 2}

    SciTech Connect (OSTI)

    TISSOT JR.,RALPH G.; RODRIGUEZ,MARK A.; SIPOLA,DIANA L.; VOIGT,JAMES A.

    2000-12-19

    Palmierite (K{sub 2}Pb(SO{sub 4}){sub 2}) has been prepared via a chemical synthesis method. Intensity differences were observed when X-ray powder data from the newly synthesized compound were compared to the published powder diffraction card (PDF) 29-1015 for Palmierite. Investigation of these differences indicated the possibility of preferred orientation and/or chemical inhomogeneity affecting intensities, particularly those of the basal (00{ell}) reflections. Annealing of the Palmierite was found to reduce the effects of preferred orientation. Electron microprobe analysis confirmed K:Pb:S as 2:1:2 for the annealed Palmierite powder. Subsequent least-squares refinement and Rietveld analysis of the annealed powder showed peak intensities very close to that of a calculated Palmierite pattern (based on single crystal data), yet substantially higher than many of the PDF 29-1015 published intensities. Further investigation of peak intensity variation via calculated patterns suggested that the intensity discrepancies between the annealed sample and those found in PDF 29-1015 were potentially due to chemical variation in the K{sub 2}Pb(SO{sub 4}){sub 2} composition. X-ray powder diffraction and crystal data for Palmierite are reported for the annealed sample. Palmierite is Trigonal/Hexagonal with unit cell parameters a = 5.497(1){angstrom}, c = 20.864(2) {angstrom}, space group R-3m (166), and Z = 3.

  9. Diamonds in the rough: a strong case for the inclusion of weak-intensity X-ray diffraction data

    SciTech Connect (OSTI)

    Wang, Jimin; Wing, Richard A.

    2014-05-01

    Here, new evidence is provided to show that the inclusion of weak-intensity, high-resolution X-ray diffraction data helps to improve the quality of experimental phases by imposing proper constraints on electron-density models during noncrystallographic symmetry averaging. Overwhelming evidence exists to show that the inclusion of weak-intensity, high-resolution X-ray diffraction data helps improve the refinement of atomic models by imposing strong constraints on individual and overall temperature B factors and thus the quality of crystal structures. Some researchers consider these data to be of little value and opt to discard them during data processing, particularly at medium and low resolution, at which individual B factors of atomic models cannot be refined. Here, new evidence is provided to show that the inclusion of these data helps to improve the quality of experimental phases by imposing proper constraints on electron-density models during noncrystallographic symmetry (NCS) averaging. Using electron-density correlation coefficients as criteria, the resolution of data has successfully been extended from 3.1 to 2.5 Å resolution with redundancy-independent merging R factors from below 100% to about 310%. It is further demonstrated that phase information can be fully extracted from observed amplitudes through de novo NCS averaging. Averaging starts with uniform density inside double-shelled spherical masks and NCS matrices that are derived from bound heavy-atom clusters at the vertices of cuboctahedrally symmetric protein particles.

  10. Structural hysteresis in dragline spider silks induced by supercontraction: an X-ray fiber micro-diffraction study

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Sampath, Sujatha; Yarger, Jeffery L.

    2014-11-27

    Interaction with water causes shrinkage and significant changes in the structure of spider dragline silks, which has been referred to as supercontraction in the literature. Preferred orientation or alignment of protein chains with respect to the fiber axis is extensively changed during this supercontraction process. Synchrotron X-ray micro-fiber diffraction experiments have been performed on Nephila clavipes and Argiope aurantia major and minor ampullate dragline spider fibers in the native dry, contracted (by immersion in water) and restretched (from contracted) states. Changes in the orientation of β-sheet nanocrystallites and the oriented component of the amorphous network have been determined from wide-anglemore » X-ray diffraction patterns. While both the crystalline and amorphous components lose preferred orientation on wetting with water, the nano-crystallites regain their orientation on wet-restretching, whereas the oriented amorphous components only partially regain their orientation. Dragline major ampullate silks in both the species contract more than their minor ampullate silks.« less

  11. Time-resolved x-ray diffraction and Raman studies of the phase transition mechanisms of methane hydrate

    SciTech Connect (OSTI)

    Hirai, Hisako Kadobayashi, Hirokazu; Hirao, Naohisa; Ohishi, Yasuo; Ohtake, Michika; Yamamoto, Yoshitaka; Nakano, Satoshi

    2015-01-14

    The mechanisms by which methane hydrate transforms from an sI to sH structure and from an sH to filled-ice Ih structure were examined using time-resolved X-ray diffractometry (XRD) and Raman spectroscopy in conjunction with charge-coupled device camera observation under fixed pressure conditions. The XRD data obtained for the sI–sH transition at 0.8 GPa revealed an inverse correlation between sI and sH, suggesting that the sI structure is replaced by sH. Meanwhile, the Raman analysis demonstrated that although the 12-hedra of sI are retained, the 14-hedra are replaced sequentially by additional 12-hedra, modified 12-hedra, and 20-hedra cages of sH. With the sH to filled-ice Ih transition at 1.8 GPa, both the XRD and Raman data showed that this occurs through a sudden collapse of the sH structure and subsequent release of solid and fluid methane that is gradually incorporated into the filled-ice Ih to complete its structure. This therefore represents a typical reconstructive transition mechanism.

  12. In situ, energy-dispersive X-ray diffraction study of natural gas conversion by CO[sub 2] reforming

    SciTech Connect (OSTI)

    Ashcroft, A.T. ); Cheetham, A.K. ); Jones, R.H.; Natarajan, S.; Thomas, J.M.; Waller, D. ); Clark, S.M. )

    1993-04-01

    The selective CO[sub 2] reforming of methane to synthesis gas over a rare-earth iridate pyrochlore, Ln[sub 2]Ir[sub 2]O[sub 7] (Ln = Eu), and rare-earth ruthenate pyrochlores, Ln[sub 2]Ru[sub 2]O[sub 7] (Ln = Nd, Sm, Eu, Gd), has been studied in situ by using energy-dispersive X-ray diffraction with synchrotron radiation. Analysis of the diffraction data shows that the oxides are activated by reduction to the platinum group metal, the iridate by a second-order kinetic reaction, and the ruthenates by a first-order process. Temperature programmed reductions under carbon monoxide, hydrogen, and methane establish that the iridates proceed directly to the metal, whereas the ruthenates reduce via an oxygen deficient pyrochlore. 18 refs., 7 figs., 1 tab.

  13. A 31?T split-pair pulsed magnet for single crystal x-ray diffraction at low temperature

    SciTech Connect (OSTI)

    Duc, F.; Frings, P.; Nardone, M.; Billette, J.; Zitouni, A.; Delescluse, P.; Bard, J.; Nicolin, J. P.; Rikken, G. L. J. A.; Fabrges, X.; Roth, T.; Detlefs, C.; Lesourd, M.; Zhang, L.

    2014-05-15

    We have developed a pulsed magnet system with panoramic access for synchrotron x-ray diffraction in magnetic fields up to 31?T and at low temperature down to 1.5?K. The apparatus consists of a split-pair magnet, a liquid nitrogen bath to cool the pulsed coil, and a helium cryostat allowing sample temperatures from 1.5 up to 250?K. Using a 1.15?MJ mobile generator, magnetic field pulses of 60?ms length were generated in the magnet, with a rise time of 16.5?ms and a repetition rate of 2 pulses/h at 31?T. The setup was validated for single crystal diffraction on the ESRF beamline ID06.

  14. Phase formation sequences in the silicon-phosphorous system : determined by in-situ synchrotron andj conventional x-ray diffraction measurements and predicted by a theoretical model.

    SciTech Connect (OSTI)

    Carlsson, J. R. A.; Clevenger, L.; Madsen, L. D.; Hultman, L.; Li, X.-H.; Jordan-Sweet, J.; Lavoie, C.; Roy, R. A.; Cabral, C., Jr.; Morales, G.; Ludwig, K. L.; Stephenson, G. B.; Hentzell, H. T. G.; Materials Science Division; Linkoeping Univ.; IBM T. J. Watson Research Center; Boston Univ.

    1997-01-01

    The phase formation sequences of Si-P alloy thin films with P concentrations between 20 and 44 at. % have been studied. The samples were annealed at progressively higher temperatures and the newly formed phases were identified both after each annealing step by ex-situ conventional X-ray diffraction (XRD) and continuously by in-situ synchrotron XRD. It was found that Si was the only phase to form in a sample with 20 at.% P since the evaporation of P at the crystallization temperature prevented phosphides from forming. For a sample with 30at.% P, the Si{sub 12}P{sub 5} phase formed prior to the SiP phase. For samples with 35 and 44at.%P, the formation of SiP preceded the formation of the Si{sub 12}P{sub 5} phase. The experimentally determined phase formation sequences were successfully predicted by a proposed model. According to the model, the first and second crystalline phases to form are those with the lowest and next-lowest crystallization temperatures of the competing compounds predicted by the Gibbs free-energy diagram.

  15. A grating-based single-shot x-ray phase contrast and diffraction method for in vivo imaging

    SciTech Connect (OSTI)

    Bennett, Eric E.; Kopace, Rael; Stein, Ashley F.; Wen Han

    2010-11-15

    Purpose: The purpose of this study is to develop a single-shot version of the grating-based phase contrast x-ray imaging method and demonstrate its capability of in vivo animal imaging. Here, the authors describe the principle and experimental results. They show the source of artifacts in the phase contrast signal and optimal designs that minimize them. They also discuss its current limitations and ways to overcome them. Methods: A single lead grid was inserted midway between an x-ray tube and an x-ray camera in the planar radiography setting. The grid acted as a transmission grating and cast periodic dark fringes on the camera. The camera had sufficient spatial resolution to resolve the fringes. Refraction and diffraction in the imaged object manifested as position shifts and amplitude attenuation of the fringes, respectively. In order to quantify these changes precisely without imposing a fixed geometric relationship between the camera pixel array and the fringes, a spatial harmonic method in the Fourier domain was developed. The level of the differential phase (refraction) contrast as a function of hardware specifications and device geometry was derived and used to guide the optimal placement of the grid and object. Both ex vivo and in vivo images of rodent extremities were collected to demonstrate the capability of the method. The exposure time using a 50 W tube was 28 s. Results: Differential phase contrast images of glass beads acquired at various grid and object positions confirmed theoretical predictions of how phase contrast and extraneous artifacts vary with the device geometry. In anesthetized rats, a single exposure yielded artifact-free images of absorption, differential phase contrast, and diffraction. Differential phase contrast was strongest at bone-soft tissue interfaces, while diffraction was strongest in bone. Conclusions: The spatial harmonic method allowed us to obtain absorption, differential phase contrast, and diffraction images, all from a

  16. InSitu X-Ray Diffraction Studies on Lithium-Ion Battery Cathodes

    SciTech Connect (OSTI)

    Doughty, Daniel H.; Ingersoll, David; Rodriguez, Mark A.

    1999-07-13

    LiNi{sub 0.8}Co{sub 0.2}O{sub 2} and LiNiO{sub 2} have been characterized in-situ XRD. LiNi{sub 0.8}Co{sub 0.2}O{sub 2} does not undergo a monoclinic phase transformation but remains a hexagonal lattice throughout the entire charging cycle. It is hypothesized that Co-doping may help stabilize the hexagonal structure.

  17. History and Solution of the Phase Problem in theTheory of Structure Determination of Crystals from X-ray Diffraction Experiments

    ScienceCinema (OSTI)

    Wolf, Emil [University of Rochester, Rochester, New York, United States

    2010-09-01

    Since the pioneering work of Max von Laue on interference and diffraction of x-rays, carried out almost 100 years ago, numerous attempts have been made to determine structures of crystalline media from x-ray diffraction experiments. The usefulness of all of them has been limited by the inability of measuring phases of the diffracted beams. In this talk, the most important research carried out in this field will be reviewed and a recently obtained solution of the phase problem will be presented.

  18. Tuning of colossal dielectric constant in gold-polypyrrole composite nanotubes using in-situ x-ray diffraction techniques

    SciTech Connect (OSTI)

    Sarma, Abhisakh; Sanyal, Milan K.

    2014-09-15

    In-situ x-ray diffraction technique has been used to study the growth process of gold incorporated polypyrrole nanotubes that exhibit colossal dielectric constant due to existence of quasi-one-dimensional charge density wave state. These composite nanotubes were formed within nanopores of a polycarbonate membrane by flowing pyrrole monomer from one side and mixture of ferric chloride and chloroauric acid from other side in a sample cell that allows collection of x-ray data during the reaction. The size of the gold nanoparticle embedded in the walls of the nanotubes was found to be dependent on chloroauric acid concentration for nanowires having diameter more than 100 nm. For lower diameter nanotubes the nanoparticle size become independent of chloroauric acid concentration and depends on the diameter of nanotubes only. The result of this study also shows that for 50 nm gold-polypyrrole composite nanotubes obtained with 5.3 mM chloroauric acid gives colossal dielectric constant of about 10{sup 7}. This value remain almost constant over a frequency range from 1Hz to 10{sup 6} Hz even at 80 K temperature.

  19. X-ray Diffraction and Multi-Frame Phase Contrast Imaging Diagnostics for IMPULSE at the Advanced Photon Source

    SciTech Connect (OSTI)

    Iverson, Adam; Carlson, Carl; Young, Jason; Curtis, Alden; Jensen, Brian; Ramos, Kyle; Yeager, John; Montgomery, David; Fezza, Kamel

    2013-07-08

    The diagnostic needs of any dynamic loading platform present unique technical challenges that must be addressed in order to accurately measure in situ material properties in an extreme environment. The IMPULSE platform (IMPact system for Ultrafast Synchrotron Experiments) at the Advanced Photon Source (APS) is no exception and, in fact, may be more challenging, as the imaging diagnostics must be synchronized to both the experiment and the 60 ps wide x-ray bunches produced at APS. The technical challenges of time-resolved x-ray diffraction imaging and high-resolution multi-frame phase contrast imaging (PCI) are described in this paper. Example data from recent IMPULSE experiments are shown to illustrate the advances and evolution of these diagnostics with a focus on comparing the performance of two intensified CCD cameras and their suitability for multi-frame PCI. The continued development of these diagnostics is fundamentally important to IMPULSE and many other loading platforms and will benefit future facilities such as the Dynamic Compression Sector at APS and MaRIE at Los Alamos National Laboratory.

  20. Mechanisms Determining the Structure of Gold-Catalyzed GaAs Nanowires Studied by in Situ X-ray Diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Takahasi, Masamitu; Kozu, Miwa; Sasaki, Takuo; Hu, Wen

    2015-09-02

    The evolution of polytypism during GaAs nanowire growth was investigated with in situ X-ray diffraction. The growth of nanowires was found to start with the formation of zincblende structure, followed by the growth of wurtzite structure. The growth process was well reproduced by a simulation based on a layer-by-layer nucleation model. The good agreement between the measured and simulated results confirms that nucleation costs higher energy for the stackings changing the crystal structure than for those conserving the preceding structure. The transition in prevalent structure can be accounted for by the change of local growth conditions related to the shapemore » of triple phase line rather than by the change in supersaturation level, which quickly reaches steady state after starting growth.« less

  1. Mechanisms Determining the Structure of Gold-Catalyzed GaAs Nanowires Studied by in Situ X-ray Diffraction

    SciTech Connect (OSTI)

    Takahasi, Masamitu; Kozu, Miwa; Sasaki, Takuo; Hu, Wen

    2015-09-02

    The evolution of polytypism during GaAs nanowire growth was investigated with in situ X-ray diffraction. The growth of nanowires was found to start with the formation of zincblende structure, followed by the growth of wurtzite structure. The growth process was well reproduced by a simulation based on a layer-by-layer nucleation model. The good agreement between the measured and simulated results confirms that nucleation costs higher energy for the stackings changing the crystal structure than for those conserving the preceding structure. The transition in prevalent structure can be accounted for by the change of local growth conditions related to the shape of triple phase line rather than by the change in supersaturation level, which quickly reaches steady state after starting growth.

  2. Time-resolved x-ray diffraction and electrical resistance measurements of structural phase transitions in zirconium

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Velisavljevic, N.; Sinogeikin, S.; Saavedra, R.; Chellappa, R. S.; Rothkirch, A.; Dattelbaum, D. M.; Konopkova, Z.; Liermann, H. -P.; Bishop, M.; Tsoi, G. M.; et al

    2014-05-07

    Here, we have designed a portable pressure controller module to tune compression rates and maximum pressures attainable in a standard gas-membrane diamond anvil cell (DAC). During preliminary experiments, performed on zirconium (Zr) metal sample, pressure jumps of up to 80 GPa were systematically obtained in less than 0.2s (resulting in compression rate of few GPa/s up to more than 400 GPa/s). In-situ x-ray diffraction and electrical resistance measurements were performed simultaneously during this rapid pressure increase to provide the first time resolved data on α → ω → β structural evolution in Zr at high pressures. Direct control of compressionmore » rates and peak pressures, which can be held for prolonged time, allows for investigation of structural evolution and kinetics of structural phase transitions of materials under previously unexplored compression rate-pressure conditions that bridge traditional static and shock/dynamic experimental platforms.« less

  3. X-ray diffraction and electron microscope studies of yttria stabilized zirconia (YSZ) ceramic coatings exposed to vanadia. Master's thesis

    SciTech Connect (OSTI)

    Kondos, K.G.

    1992-09-01

    The U.S. Navy sometimes has the requirement to use low cost fuels containing significant amounts of vanadium and sulfur in gas turbine engines. Unfortunately the yttria stabilized zirconia (YSZ) witch is used as a thermal barrier coating on gas turbine blades can be severely attacked by vanadia. Powders of YSZ containing 8-mol% Y203 and pure zirconia containing various and mounts Of V205 were annealed at 900 deg. C. These were then examined by X-ray diffraction and electron microscopy, as well as single crystals of pure Zro2 and YSZ ( 20% Wt Y203 ) exposed to V205 Melts, to study how the vanadia degrades the YSZ by reacting with the stabilizer to form YVO4 and how the vanadium transforms the cubic and tetragonal YSZ crystal structures to monoclinic which degrades rapidly as a gas turbine blade coating.

  4. Frustrated smectic layer structures in bent-shaped dimer liquid crystals studied by x-ray microbeam diffraction

    SciTech Connect (OSTI)

    Takanishi, Yoichi; Toshimitsu, Megumi; Nakata, Michi; Takada, Naoki; Izumi, Tatsuya; Ishikawa, Ken; Takezoe, Hideo; Watanabe, Junji; Takahashi, Yumiko; Iida, Atsuo

    2006-11-15

    The layer structures in bent-shaped liquid crystal dimers mOAM5AMOm (m=6-16) have been investigated by x-ray microbeam diffraction. These liquid crystal molecules have two rodlike mesogens connected with an odd-numbered alkylene spacer and form a bent shape. In these compounds it is found that the structure changes from the single (m=6) to frustrated-layer structures (m=8, 10, and 12) and switchable frustrated-layer structures (m=14 and 16) with increasing terminal chain length. An anticlinic antiferroelectric structure is suggested in the compound with m=16, based on the different electric-field-induced reorientation behavior from those in the other dimers.

  5. Synthesis and single crystal x-ray diffraction study of a Schiff base derived from 4-acylpyrazolone and 2-aminophenol

    SciTech Connect (OSTI)

    Sharma, Naresh; Kant, Rajni Gupta, Vivek K.; Jadeja, R. N.

    2014-04-24

    The title compound, (Z)-1-(3-chlorophenyl)-4[1((2hydroxyphenyl)amino)propylidene] -3-methyl-1H-pyrazol-5(4H)-one was synthesized by refluxing compound 1-(m-chlorophenyl)-3-methyl-4-propionyl-5-pyrazolone, with 2-aminophenol in ethanol. The compound crystallizes in the orthorhombic crystal system with space group Pca2{sub 1} having unit cell parameters: a = 26.2993(8), b = 7.0724(2) and c = 18.7170(5)Å. The structure contains two crystallographically independent molecules, A, and, B, in the asymmetric unit cell. The crystal structure was solved by direct method using single crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R- value of 0.049 for 5207 observed reflections.

  6. Thermoelastic study of nanolayered structures using time-resolved X-ray diffraction at high repetition rate

    SciTech Connect (OSTI)

    Navirian, H. A.; Schick, D. Leitenberger, W.; Bargheer, M.; Gaal, P.; Shayduk, R.

    2014-01-13

    We investigate the thermoelastic response of a nanolayered sample composed of a metallic SrRuO{sub 3} electrode sandwiched between a ferroelectric Pb(Zr{sub 0.2}Ti{sub 0.8})O{sub 3} film with negative thermal expansion and a SrTiO{sub 3} substrate. SrRuO{sub 3} is rapidly heated by fs-laser pulses with 208?kHz repetition rate. Diffraction of X-ray pulses derived from a synchrotron measures the transient out-of-plane lattice constant c of all three materials simultaneously from 120?ps to 5??s with a relative accuracy up to ?c/c?=?10{sup ?6}. The in-plane propagation of sound is essential for understanding the delayed out-of-plane compression of Pb(Zr{sub 0.2}Ti{sub 0.8})O{sub 3}.

  7. {ital In} {ital situ} x-ray diffraction analysis of the C49--C54 titanium silicide phase transformation in narrow lines

    SciTech Connect (OSTI)

    Roy, R.A.; Clevenger, L.A.; Cabral, C. Jr.; Saenger, K.L.; Brauer, S.; Jordan-Sweet, J.; Bucchignano, J.; Stephenson, G.B.; Morales, G.; Ludwig, K.F. Jr.

    1995-04-03

    The transformation of titanium silicide from the C49 to the C54 structure was studied using x-ray diffraction of samples containing arrays of narrow lines of preformed C49 TiSi{sub 2}. Using a synchrotron x-ray source, diffraction patterns were collected at 1.5--2 {degree}C intervals during sample heating at rates of 3 or 20 {degree}C/s to temperatures of 1000--1100 {degree}C. The results show a monotonic increase in the C54 transition temperature by as much as 180 {degree}C with a decreasing linewidth from 1.0 to 0.1 {mu}m. Also observed is a monotonic increase in (040) preferred orientation of the C54 phase with decreasing linewidth. The results demonstrate the power of {ital in} {ital situ} x-ray diffraction of narrow line arrays as a tool to study finite size effects in thin-film reactions.

  8. Neutron diffraction and X-ray absorption study of Ag{sub 5}Pb{sub 2}O{sub 6}

    SciTech Connect (OSTI)

    Yoshii, K. Mizumaki, M.; Kato, K.; Uruga, T.; Abe, H.; Nakamura, A.; Shimojo, Y.; Ishii, Y.; Morii, Y.

    2007-01-15

    Neutron diffraction and X-ray absorption measurements were carried out for a silver-lead oxide Ag{sub 5}Pb{sub 2}O{sub 6}. The powder neutron diffraction patterns could be fitted to the trigonal P3-bar 1m structure, as was found by X-ray diffraction. From the bond-valence-sum (BVS) analysis, the valences of the Ag and Pb ions were estimated to be about 1+ and 3.7+, respectively. The X-ray absorption measurements indicated that the ionic state of Ag is close to 1+, while that of Pb stands between 3+ and 4+. The deviation of the valence of the Pb ion from 4+ suggests a contribution of Pb orbitals to the metallic conduction as well as the possible superconductivity of this material, consistently with a recent band-structure calculation.

  9. Near-surface density profiling of Fe ion irradiated Si (100) using extremely asymmetric x-ray diffraction by variation of the wavelength

    SciTech Connect (OSTI)

    Khanbabaee, B. Pietsch, U.; Facsko, S.; Doyle, S.

    2014-10-20

    In this work, we report on correlations between surface density variations and ion parameters during ion beam-induced surface patterning process. The near-surface density variations of irradiated Si(100) surfaces were investigated after off-normal irradiation with 5 keV Fe ions at different fluences. In order to reduce the x-ray probing depth to a thickness below 5?nm, the extremely asymmetrical x-ray diffraction by variation of wavelength was applied, exploiting x-ray refraction at the air-sample interface. Depth profiling was achieved by measuring x-ray rocking curves as function of varying wavelengths providing incidence angles down to 0. The density variation was extracted from the deviations from kinematical Bragg angle at grazing incidence angles due to refraction of the x-ray beam at the air-sample interface. The simulations based on the dynamical theory of x-ray diffraction revealed that while a net near-surface density decreases with increasing ion fluence which is accompanied by surface patterning, there is a certain threshold of ion fluence to surface density modulation. Our finding suggests that the surface density variation can be relevant with the mechanism of pattern formation.

  10. Purification, crystallization and preliminary X-ray diffraction analysis of the plant Rho protein ROP5

    SciTech Connect (OSTI)

    Thomas, Christoph Berken, Antje

    2007-12-01

    Crystals of the plant Rho protein ROP5 from A. thaliana have been obtained that diffract to 1.53 resolution. The small G protein ROP5 from the model plant Arabidopsis thaliana was purified and crystallized using the hanging-drop vapour-diffusion method. ROP5 crystals were obtained using PEG 3000 as precipitant and belong to space group P2{sub 1}. A data set was collected to 1.53 resolution using synchrotron radiation at 100 K. A clear molecular-replacement solution was found using ROP4GDP of the ROP4GDPPRONE8 complex as the search model.

  11. The Crystal Structure of Thorium and Zirconium Dihydrides by X-ray and Neutron Diffraction

    DOE R&D Accomplishments [OSTI]

    Rundle, R.E.; Shull, C.G.; Wollan, E.O.

    1951-04-20

    Thorium forms a tetragonal lower hydride of composition ThH{sub 2}. The hydrides ThH{sub 2}, ThD{sub 2}, and ZrD{sub 2} have been studied by neutron diffraction in order that hydrogen positions could be determined. The hydrides are isomorphous, and have a deformed fluorite structure. Metal-hydrogen distances in thorium hydride are unusually large, as in UH{sub 3}. Thorium and zirconium scattering amplitudes and a revised scattering amplitude for deuterium are reported.

  12. A facility for X-ray diffraction in magnetic fields up to 25 T and temperatures between 15 and 295 K

    SciTech Connect (OSTI)

    Wang, S.; Kovalev, A. E. Suslov, A. V.; Siegrist, T.

    2015-12-15

    A facility for X-ray diffraction has been developed at the National High Magnetic Field Laboratory. It brings diffraction capability to the 25 T Florida split coil magnet and implements temperature control in a range of 15–295 K using a cold finger helium cryostat. This instrument represents an alternative to pulsed magnetic field systems, and it exceeds the static magnetic fields currently available at synchrotron facilities. Magnetic field compatibility of an X-ray source and detectors with the sizable magnetic fringe fields emanating from the magnet constrained the design of the diffractometer.

  13. Characterization of beryllium deformation using in-situ x-ray diffraction

    SciTech Connect (OSTI)

    Magnuson, Eric Alan; Brown, Donald William; Clausen, Bjorn; Sisneros, Thomas A.; Park, Jun-Sang

    2015-08-24

    Beryllium’s unique mechanical properties are extremely important in a number of high performance applications. Consequently, accurate models for the mechanical behavior of beryllium are required. However, current models are not sufficiently microstructure aware to accurately predict the performance of beryllium under a range of processing and loading conditions. Previous experiments conducted using the SMARTS and HIPPO instruments at the Lujan Center(LANL), have studied the relationship between strain rate and texture development, but due to the limitations of neutron diffraction studies, it was not possible to measure the response of the material in real-time. In-situ diffraction experiments conducted at the Advanced Photon Source have allowed the real time measurement of the mechanical response of compressed beryllium. Samples of pre-strained beryllium were reloaded orthogonal to their original load path to show the reorientation of already twinned grains. Additionally, the in-situ experiments allowed the real time tracking of twin evolution in beryllium strained at high rates. The data gathered during these experiments will be used in the development and validation of a new, microstructure aware model of the constitutive behavior of beryllium.

  14. Direct observation of intrinsic piezoelectricity of Pb(Zr,Ti)O{sub 3} by time-resolved x-ray diffraction measurement using single-crystalline films

    SciTech Connect (OSTI)

    Fujisawa, Takashi; Ehara, Yoshitaka; Yasui, Shintaro; Kamo, Takafumi; Funakubo, Hiroshi; Yamada, Tomoaki; Sakata, Osami

    2014-07-07

    Lead zirconate titanate, Pb(Zr,Ti)O{sub 3} or PZT, is one of the most widely investigated ferroelectric and piezoelectric materials due to its superior properties. However, the intrinsic properties of PZT have not been directly measured due to the lack of fabrication of single crystals even though a basic understanding of intrinsic properties has been of interest developing lead-free piezoelectric materials. We demonstrated the direct observation of the intrinsic piezoelectric property by means of the detection of electric-field induced crystal lattice distortion of thick Pb(Zr{sub 0.35}Ti{sub 0.65})O{sub 3} single-crystalline films with single polar-axis orientation and negligible residual strain using the time-resolved X-ray diffraction (XRD) together with the polarization response. Consequently, the effective converse piezoelectric response was experimentally revealed; hence, the electrostrictive coefficient, which is the conversion coefficient between the electrical and mechanical response, was determined. The obtained effective electrostrictive coefficient was 5.2–6.3 × 10{sup −2} m{sup 4}/C{sup 2}, which agrees with theoretical prediction.

  15. X-ray diffraction and Raman scattering study of Cr-doped ZnFe{sub 2}O{sub 4} spinel ferrites

    SciTech Connect (OSTI)

    Kumar, Ashwini; Sharma, Poorva; Varshney, Dinesh

    2015-06-24

    XRD and Raman scattering measurements were made on polycrystalline ZnFe{sub 2-x}Cr{sub x}O{sub 4} (x=0.0, 0.1, 0.2) spinel ferrites as prepared by solid-state reaction route. Rietveld refined X-ray diffraction pattern confirmed the formation of single-phase and are indexed in cubic structure with Fd3m space group. Slight reduction in the lattice parameter from 8.435 to 8.410 Ǻ, with Cr{sup 3+} ion substitution has been observed. From Raman scattering spectra, the modes of ZnFe{sub 1.9}Cr{sub 0.1}O{sub 4} and ZnFe{sub 1.8}Cr{sub 0.2}O{sub 4} are shifted towards the lower frequency side as compared to ZnFe{sub 2}O{sub 4}, this red shift is attributed to higher atomic mass of Zn (65.39 amu) as compared to Fe (55.84 amu)

  16. Purification, crystallization and preliminary X-ray diffraction of human S100A15

    SciTech Connect (OSTI)

    Boeshans, Karen M.; Wolf, Ronald; Voscopoulos, Christopher; Gillette, William; Esposito, Dominic; Mueser, Timothy C.; Yuspa, Stuart H.; Ahvazi, Bijan

    2006-05-01

    S100 proteins are differentially expressed during epithelial cell maturation, tumorigenesis and inflammation. The novel human S100A15 protein has been cloned, expressed, purified and crystallized in two crystal forms, a triclinic and a monoclinic form, which diffract to 1.7 and 2.0 Å, respectively. Human S100A15 is a novel member of the S100 family of EF-hand calcium-binding proteins and was recently identified in psoriasis, where it is significantly upregulated in lesional skin. The protein is implicated as an effector in calcium-mediated signal transduction pathways. Although its biological function is unclear, the association of the 11.2 kDa S100A15 with psoriasis suggests that it contributes to the pathogenesis of the disease and could provide a molecular target for therapy. To provide insight into the function of S100A15, the protein was crystallized to visualize its structure and to further the understanding of how the many similar calcium-binding mediator proteins in the cell distinguish their cognate target molecules. The S100A15 protein has been cloned, expressed and purified to homogeneity and produced two crystal forms. Crystals of form I are triclinic, with unit-cell parameters a = 33.5, b = 44.3, c = 44.8 Å, α = 71.2, β = 68.1, γ = 67.8° and an estimated two molecules in the asymmetric unit, and diffract to 1.7 Å resolution. Crystals of form II are monoclinic, with unit-cell parameters a = 82.1, b = 33.6, c = 52.2 Å, β = 128.2° and an estimated one molecule in the asymmetric unit, and diffract to 2.0 Å resolution. This structural analysis of the human S100A15 will further aid in the phylogenic comparison between the other members of the S100 protein family, especially the highly homologous paralog S100A7.

  17. Crystallization and preliminary X-ray diffraction analysis of the small laccase from Streptomyces coelicolor

    SciTech Connect (OSTI)

    Skálová, Tereza; Dohnálek, Jan; Østergaard, Lars Henrik; Østergaard, Peter Rahbek

    2007-12-01

    The expression, purification and crystallization of the small laccase from S. coelicolor are reported. Diffraction data were collected to 3 Å resolution. The small bacterial laccase from the actinobacterium Streptomyces coelicolor which lacks the second of the three domains of the laccases structurally characterized to date was crystallized. This multi-copper phenol oxidase crystallizes in a primitive tetragonal lattice, with unit-cell parameters a = b = 179.8, c = 175.3 Å. The crystals belong to either space group P4{sub 1}2{sub 1}2 or P4{sub 3}2{sub 1}2. The self-rotation function shows the presence of a noncrystallographic threefold axis in the structure. Phases will be determined from the anomalous signal of the natively present copper ions.

  18. High-resolution x-ray diffraction study of the heavy-fermion compound YbBiPt

    SciTech Connect (OSTI)

    Ueland, B. G.; Saunders, S. M.; Bud'ko, S. L.; Schmiedeshoff, G. M.; Canfield, P. C.; Kreyssig, A.; Goldman, A. I.

    2015-11-30

    In this study, YbBiPt is a heavy-fermion compound possessing significant short-range antiferromagnetic correlations below a temperature of T*=0.7K, fragile antiferromagnetic order below TN = 0.4K, a Kondo temperature of TK ? 1K, and crystalline-electric-field splitting on the order of E/kB = 1 10K. Whereas the compound has a face-centered-cubic lattice at ambient temperature, certain experimental data, particularly those from studies aimed at determining its crystalline-electric-field scheme, suggest that the lattice distorts at lower temperature. Here, we present results from high-resolution, high-energy x-ray diffraction experiments which show that, within our experimental resolution of ? 6 10 105 , no structural phase transition occurs between T = 1.5 and 50 K. In combination with results from dilatometry measurements, we further show that the compound's thermal expansion has a minimum at ? 18 K and a region of negative thermal expansion for 9 ? T ? 18 K. Despite diffraction patterns taken at 1.6 K which indicate that the lattice is face-centered cubic and that the Yb resides on a crystallographic site with cubic point symmetry, we demonstrate that the linear thermal expansion may be modeled using crystalline-electric-field level schemes appropriate for Yb3+ residing on a site with either cubic or less than cubic point symmetry.

  19. Reconstruction of a yeast cell from x-ray diffraction data

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Thibault, Pierre; Elser, Veit; Jacobsen, Chris; Shapiro, David; Sayre, David

    2006-06-21

    We provide details of the algorithm used for the reconstruction of yeast cell images in the recent demonstration of diffraction microscopy by Shapiro, Thibault, Beetz, Elser, Howells, Jacobsen, Kirz, Lima, Miao, Nieman & Sayre. Two refinements of the iterative constraint-based scheme are developed to address the current experimental realities of this imaging technique, which include missing central data and noise. A constrained power operator is defined whose eigenmodes allow the identification of a small number of degrees of freedom in the reconstruction that are negligibly constrained as a result of the missing data. To achieve reproducibility in the algorithm's output,more » a special intervention is required for these modes. Weak incompatibility of the constraints caused by noise in both direct and Fourier space leads to residual phase fluctuations. This problem is addressed by supplementing the algorithm with an averaging method. The effect of averaging may be interpreted in terms of an effective modulation transfer function, as used in optics, to quantify the resolution. The reconstruction details are prefaced with simulations of wave propagation through a model yeast cell. These show that the yeast cell is a strong-phase-contrast object for the conditions in the experiment.« less

  20. Revisiting the blocking force test on ferroelectric ceramics using high energy x-ray diffraction

    SciTech Connect (OSTI)

    Daniel, L.; Hall, D. A.; Withers, P. J.; Koruza, J.; Webber, K. G.; King, A.

    2015-05-07

    The blocking force test is a standard test to characterise the properties of piezoelectric actuators. The aim of this study is to understand the various contributions to the macroscopic behaviour observed during this experiment that involves the intrinsic piezoelectric effect, ferroelectric domain switching, and internal stress development. For this purpose, a high energy diffraction experiment is performed in-situ during a blocking force test on a tetragonal lead zirconate titanate (PZT) ceramic (Pb{sub 0.98}Ba{sub 0.01}(Zr{sub 0.51}Ti{sub 0.49}){sub 0.98}Nb{sub 0.02}O{sub 3}). It is shown that the usual macroscopic linear interpretation of the test can also be performed at the single crystal scale, allowing the identification of local apparent piezoelectric and elastic properties. It is also shown that despite this apparent linearity, the blocking force test involves significant non-linear behaviour mostly due to domain switching under electric field and stress. Although affecting a limited volume fraction of the material, domain switching is responsible for a large part of the macroscopic strain and explains the high level of inter- and intra-granular stresses observed during the course of the experiment. The study shows that if apparent piezoelectric and elastic properties can be identified for PZT single crystals from blocking stress curves, they may be very different from the actual properties of polycrystalline materials due to the multiplicity of the physical mechanisms involved. These apparent properties can be used for macroscopic modelling purposes but should be considered with caution if a local analysis is aimed at.

  1. Synchrotron X-ray diffraction studies of phase transitions and mechanical properties of nanocrystalline materials at high pressure

    SciTech Connect (OSTI)

    Prilliman, Gerald Stephen

    2003-09-01

    The behavior of nanocrystals under extreme pressure was investigated using synchrotron x-ray diffraction. A major part of this investigation was the testing of a prototype synchrotron endstation on a bend magnet beamline at the Advanced Light Source for high pressure work using a diamond anvil cell. The experiments conducted and documented here helped to determine issues of efficiency and accuracy that had to be resolved before the construction of a dedicated ''super-bend'' beamline and endstation. The major conclusions were the need for a cryo-cooled monochromator and a fully remote-controllable pressurization system which would decrease the time to change pressure and greatly reduce the error created by the re-placement of the diamond anvil cell after each pressure change. Two very different types of nanocrystal systems were studied, colloidal iron oxide (Fe{sub 2}O{sub 3}) and thin film TiN/BN. Iron oxide nanocrystals were found to have a transition from the {gamma} to the {alpha} structure at a pressure strongly dependent on the size of the nanocrystals, ranging from 26 GPa for 7.2 nm nanocrystals to 37 GPa for 3.6 nm nanocrystals. All nanocrystals were found to remain in the {alpha} structure even after release of pressure. The transition pressure was also found, for a constant size (5.7 nm) to be strongly dependent on the degree of aggregation of the nanocrystals, increasing from 30 GPa for completely dissolved nanocrystals to 45 GPa for strongly aggregated nanocrystals. Furthermore, the x-ray diffraction pattern of the pressure induced {alpha} phase demonstrated a decrease in intensity for certain select peaks. Together, these observations were used to make a complete picture of the phase transition in nanocrystalline systems. The size dependence of the transition was interpreted as resulting from the extremely high surface energy of the {alpha} phase which would increase the thermodynamic offset and thereby increase the kinetic barrier to transition that

  2. Petrographic and X-ray diffraction analyses of selected samples from Marker Bed 139 at the Waste Isolation Pilot Plant

    SciTech Connect (OSTI)

    Fredrich, J.T.; Zeuch, D.H.

    1996-04-01

    The Waste Isolation Pilot Plant (WIPP) is located 660 m underground in the Salado Formation which consists of thick, horizontally bedded pure and impure salt and thin, laterally continuous clay and anhydrite interbeds. The Salado Two-Phase Flow Laboratory Program was established to provide site-specific-two-phase flow and other related rock properties to support performance assessment modeling of the WIPP repository. Owing to their potentially significant role in the hydrologic response of the repository, the program initially focused on the anhydrite interbeds, and in particular, on Marker Bed 139 (MB 139), which lies approximately 1 m below the planned waste storage rooms. This report synthesizes petrographic and X-ray powder diffraction studies performed to support the Salado Two-Phase Flow Laboratory Program. Experimental scoping activities in this area were performed in FY 1993 by three independent laboratories in order to: (1) quantify the mineral composition to support laboratory studies of hydrologic properties and facilitate correlation of transport properties with composition; (2) describe textures, including grain size; and (3) describe observed porosity. Samples from various depths were prepared from six 6-inch diameter cores which were obtained by drilling into the marker bed from the floor of two separate rooms. The petrographic analyses are augmented here with additional study of the original thin sections, and the pore structure observations are also examined in relation to an independent observational study of microcracks in Marker Bed 139 core samples performed in FY 1994 by the Geomechanics Department at Sandia National Laboratories.

  3. Ferrocyanide Safety Project Dynamic X-Ray Diffraction studies of sodium nickel ferrocyanide reactions with equimolar nitrate/nitrite salts

    SciTech Connect (OSTI)

    Dodds, J.N. |

    1994-07-01

    Dynamic X-ray Diffraction (DXRD) has been to used to identify and quantify the solid state reactions that take place between sodium nickel ferrocyanide, Na{sub 2}NiFe(CN){sub 6}, and equimolar concentrations of sodium nitrate/nitrite, reactions of interest to the continued environmental safety of several large underground waste storage tanks at the Hanford site in eastern Washington. The results are supportive of previous work, which indicated that endothermic dehydration and melting of the nitrates take place before the occurrence of exothermic reactions that being about 300{degrees}C. The DXRD results show that a major reaction set at these temperatures is the occurrence of a series reaction that produces sodium cyanate, NaCNO, as an intermediate in a mildly exothermic first step. In the presence of gaseous oxygen, NaCNO subsequently reacts exothermally and at a faster rate to form metal oxides. Measurements of the rate of this reaction are used to estimate the heat release. Comparisons of this estimated heat release rate with heat transfer rates from a hypothetical ``hot spot`` show that, even in a worst-case scenario, the heat transfer rates are approximately eight times higher than the rate of energy release from the exothermic reactions.

  4. In situ X-ray diffraction and the evolution of polarization during the growth of ferroelectric superlattices

    SciTech Connect (OSTI)

    Bein, Benjamin; Hsing, Hsiang-Chun; Callori, Sara J.; Sinsheimer, John; Chinta, Priya V.; Headrick, Randall L.; Dawber, Matthew

    2015-12-04

    In the epitaxially strained ferroelectric thin films and superlattices, the ferroelectric transition temperature can lie above the growth temperature. Ferroelectric polarization and domains should then evolve during the growth of a sample, and electrostatic boundary conditions may play an important role. In this work, ferroelectric domains, surface termination, average lattice parameter and bilayer thickness are simultaneously monitored using in situ synchrotron X-ray diffraction during the growth of BaTiO3/SrTiO3 superlattices on SrTiO3 substrates by off-axis radio frequency magnetron sputtering. The technique used allows for scan times substantially faster than the growth of a single layer of material. Effects of electric boundary conditions are investigated by growing the same superlattice alternatively on SrTiO3 substrates and 20 nm SrRuO3 thin films on SrTiO3 substrates. Our experiments provide important insights into the formation and evolution of ferroelectric domains when the sample is ferroelectric during the growth process.

  5. In situ X-ray diffraction and the evolution of polarization during the growth of ferroelectric superlattices

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Bein, Benjamin; Hsing, Hsiang-Chun; Callori, Sara J.; Sinsheimer, John; Chinta, Priya V.; Headrick, Randall L.; Dawber, Matthew

    2015-12-04

    In the epitaxially strained ferroelectric thin films and superlattices, the ferroelectric transition temperature can lie above the growth temperature. Ferroelectric polarization and domains should then evolve during the growth of a sample, and electrostatic boundary conditions may play an important role. In this work, ferroelectric domains, surface termination, average lattice parameter and bilayer thickness are simultaneously monitored using in situ synchrotron X-ray diffraction during the growth of BaTiO3/SrTiO3 superlattices on SrTiO3 substrates by off-axis radio frequency magnetron sputtering. The technique used allows for scan times substantially faster than the growth of a single layer of material. Effects of electric boundarymore » conditions are investigated by growing the same superlattice alternatively on SrTiO3 substrates and 20 nm SrRuO3 thin films on SrTiO3 substrates. Our experiments provide important insights into the formation and evolution of ferroelectric domains when the sample is ferroelectric during the growth process.« less

  6. High-resolution x-ray diffraction study of the heavy-fermion compound YbBiPt

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Ueland, B. G.; Iowa State Univ., Ames, IA; Saunders, S. M.; Iowa State Univ., Ames, IA; Bud'ko, S. L.; Iowa State Univ., Ames, IA; Schmiedeshoff, G. M.; Canfield, P. C.; Iowa State Univ., Ames, IA; Kreyssig, A.; et al

    2015-11-30

    In this study, YbBiPt is a heavy-fermion compound possessing significant short-range antiferromagnetic correlations below a temperature of T*=0.7K, fragile antiferromagnetic order below TN = 0.4K, a Kondo temperature of TK ≈ 1K, and crystalline-electric-field splitting on the order of E/kB = 1 – 10K. Whereas the compound has a face-centered-cubic lattice at ambient temperature, certain experimental data, particularly those from studies aimed at determining its crystalline-electric-field scheme, suggest that the lattice distorts at lower temperature. Here, we present results from high-resolution, high-energy x-ray diffraction experiments which show that, within our experimental resolution of ≈ 6 – 10 × 10–5 Å,more » no structural phase transition occurs between T = 1.5 and 50 K. In combination with results from dilatometry measurements, we further show that the compound's thermal expansion has a minimum at ≈ 18 K and a region of negative thermal expansion for 9 ≲ T ≲ 18 K. Despite diffraction patterns taken at 1.6 K which indicate that the lattice is face-centered cubic and that the Yb resides on a crystallographic site with cubic point symmetry, we demonstrate that the linear thermal expansion may be modeled using crystalline-electric-field level schemes appropriate for Yb3+ residing on a site with either cubic or less than cubic point symmetry.« less

  7. In situ monitoring of the electrochemical absorption of deuterium into palladium by x-ray diffraction using synchrotron-wiggler radiation

    SciTech Connect (OSTI)

    Dominguez, D.D.; Hagans, P.L.; Skelton, E.F.; Qadri, S.B.; Nagel, D.J.

    1998-12-31

    With low energy x-rays, such as those from a Cu x-ray tube, only the outer few microns of a metallic sample can be probed. This low penetrating power prohibits structural studies from being carried out on the interior of an electrode in an electrochemical cell because of absorption by the cell material, electrodes and the electrolyte. The work described in this paper circumvents this problem by utilizing high energy, high brightness x-rays produced on the superconducting wiggler beam line, X-17C, at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory. The penetrating power of the higher energy x-rays allowed Pd diffraction spectra to be obtained in-situ on a 1 mm diameter Pd wire cathode during electrolysis of heavy water. Moreover, the beam (28 x 28 {micro}m in cross-section) allowed diffraction spectra to be acquired as a function of distance across the sample. Spectra were recorded in 50 {micro}m steps from the edge of the Pd wire to its core. This was done at 2 minute intervals as a function of electrolysis time. The {alpha}-{beta} phase transition induced in the Pd while deuterium was electrochemically absorbed was observed by monitoring the Pd-(422) diffraction peaks. Results allowed the diffusion rate and the diffusivity of deuterium atoms in the Pd wire to be determined. Other features of the structural changes associated with the absorption of deuterium into Pd are reported.

  8. Characterization of the Products of the Heme Detoxification Pathway in Malarial Late Trophozoites by X-ray Diffraction

    SciTech Connect (OSTI)

    Bohle,D.; Dinnebier, R.; Madsen, S.; Stephens, P.

    2007-01-01

    detoxify heme released during the degradation of hemoglobin by aggregating it into malarial pigment, an insoluble crystalline heme coordination polymer. Synchrotron x-ray powder diffraction patterns for intact desiccated malarial trophozoites and synthetic {beta}-hematin have been measured; both materials correspond to a single crystalline triclinic lattice with unit cell parameters a = 12.2176(4), b = 14.7184(5), c = 8.0456(3) {angstrom}; {alpha} = 90.200(2), {beta} = 96.806(3), {gamma} = 97.818(3){sup o} and Z = 2. These results unambiguously demonstrate that hemozoin crystallites are identical to synthetic {beta}-hematin.

  9. High energy X-ray diffraction study of a dental ceramics–titanium functional gradient material prepared by field assisted sintering technique

    SciTech Connect (OSTI)

    Witte, K.; Bodnar, W.; Schell, N.; Lang, H.; Burkel, E.

    2014-09-15

    A functional gradient material with eleven layers composed of a dental ceramics and titanium was successfully consolidated using field assisted sintering technique in a two-step sintering process. High energy X-ray diffraction studies on the gradient were performed at High Energy Material Science beamline at Desy in Hamburg. Phase composition, crystal unit edges and lattice mismatch along the gradient were determined applying Rietveld refinement procedure. Phase analysis revealed that the main crystalline phase present in the gradient is α-Ti. Crystallinity increases stepwisely along the gradient with a decreasing increment between every next layer, following rather the weight fraction of titanium. The crystal unit edge a of titanium remains approximately constant with a value of 2.9686(1) Å, while c is reduced with increasing amount of titanium. In the layer with pure titanium the crystal unit edge c is constant with a value of 4.7174(2) Å. The lattice mismatch leading to an internal stress was calculated over the whole gradient. It was found that the maximal internal stress in titanium embedded in the studied gradient is significantly smaller than its yield strength, which implies that the structure of titanium along the whole gradient is mechanically stable. - Highlights: • High energy XRD studies of dental ceramics–Ti gradient material consolidated by FAST. • Phase composition, crystallinity and lattice parameters are determined. • Crystallinity increases stepwisely along the gradient following weight fraction of Ti. • Lattice mismatch leading to internal stress is calculated over the whole gradient. • Internal stress in α-Ti embedded in the gradient is smaller than its yield strength.

  10. Strain and lattice orientation distribution in SiN/Ge complementary metaloxidesemiconductor compatible light emitting microstructures by quick x-ray nano-diffraction microscopy

    SciTech Connect (OSTI)

    Chahine, G. A.; Schlli, T. U.; Zoellner, M. H.; Guha, S.; Reich, C.; Zaumseil, P.; Capellini, G.; Richard, M.-I.; Schroeder, T.

    2015-02-16

    This paper presents a study of the spatial distribution of strain and lattice orientation in CMOS-fabricated strained Ge microstripes using high resolution x-ray micro-diffraction. The recently developed model-free characterization tool, based on a quick scanning x-ray diffraction microscopy technique can image strain down to levels of 10{sup ?5} (?a/a) with a spatial resolution of ?0.5??m. Strain and lattice tilt are extracted using the strain and orientation calculation software package X-SOCS. The obtained results are compared with the biaxial strain distribution obtained by lattice parameter-sensitive ?-Raman and ?-photoluminescence measurements. The experimental data are interpreted with the help of finite element modeling of the strain relaxation dynamics in the investigated structures.

  11. Structural and chemical ordering of Heusler CoxMnyGez epitaxial films on Ge (111). Quantitative study using traditional and anomalous x-ray diffraction techniques

    SciTech Connect (OSTI)

    Collins, B. A.; Chu, Y.; He, L.; Haskel, D.; Tsui, F.

    2015-12-14

    We found that epitaxial films of CoxMnyGez grown on Ge (111) substrates by molecular-beam-epitaxy techniques have been investigated as a continuous function of composition using combinatorial synchrotron x-ray diffraction (XRD) and x-ray fluorescence (XRF) spectroscopy techniques. A high-resolution ternary epitaxial phase diagram is obtained, revealing a small number of structural phases stabilized over large compositional regions. Ordering of the constituent elements in the compositional region near the full Heusler alloy Co2MnGe has been examined in detail using both traditional XRD and a new multiple-edge anomalous diffraction (MEAD) technique. Multiple-edge anomalous diffraction involves analyzing the energy dependence of multiple reflections across each constituent absorption edge in order to detect and quantify the elemental distribution of occupation in specific lattice sites. Results of this paper show that structural and chemical ordering are very sensitive to the Co : Mn atomic ratio, such that the ordering is the highest at an atomic ratio of 2 but significantly reduced even a few percent off this ratio. The in-plane lattice is nearly coherent with that of the Ge substrate, while the approximately 2% lattice mismatch is accommodated by the out-of-plane tetragonal strain. Furthermore, the quantitative MEAD analysis reveals no detectable amount (<0.5%) of Co-Mn site swapping, but instead high levels (26%) of Mn-Ge site swapping. Increasing Ge concentration above the Heusler stoichiometry (Co 0.5 Mn 0.25 Ge 0.25 ) is shown to correlate with increased lattice vacancies, antisites, and stacking faults, but reduced lattice relaxation. The highest degree of chemical ordering is observed off the Heusler stoichiometry with a Ge enrichment of 5 at.%.

  12. Synthesis and X-ray diffraction study of palladium(II) 1,3-diphenyl-5-(benzothiazol-2-yl)formazanate

    SciTech Connect (OSTI)

    Zaidman, A. V., E-mail: biosphera@usfeu.ru; Pervova, I. G.; Rezinskikh, Z. G.; Lipunov, I. N. [Ural State Forest Engineering University (Russian Federation); Slepukhin, P. A., E-mail: slepukhin@ios.uran.ru [Russian Academy of Sciences, Postovsky Institute of Organic Synthesis, Ural Division (Russian Federation)

    2010-05-15

    The behavior of 1,3-diphenyl-5-(benzothiazol-2-yl)formazan as a bidentate ligand in the synthesis of the mononuclear palladium complex was investigated using slow diffusion. According to the X-ray diffraction study, the PdN4 coordination unit has a distorted square structure. The ligands form two six-membered chelate rings formed through the N1 and N4 atoms of the formazan fragment.

  13. A short note on physical properties to irradiated nuclear fuel by means of X-ray diffraction and neutron scattering techniques

    SciTech Connect (OSTI)

    Abdullah, Yusof Husain, Hishamuddin; Hak, Cik Rohaida Che; Alias, Nor Hayati; Yusof, Mohd Reusmaazran; Kasim, Norasiah Ab; Zali, Nurazila Mat; Mohamed, Abdul Aziz

    2015-04-29

    For nuclear reactor applications, understanding the evolution of the fuel materials microstructure during irradiation are of great importance. This paper reviews the physical properties of irradiated nuclear fuel analysis which are considered to be of most importance in determining the performance behavior of fuel. X-rays diffraction was recognize as important tool to investigate the phase identification while neutron scattering analyses the interaction between uranium and other materials and also investigation of the defect structure.

  14. Some new schemes for producing high-accuracy elliptical X-ray mirrors by elastic bending

    SciTech Connect (OSTI)

    Padmore, H.A.; Howells, M.R.; Irick, S.; Renner, T.; Sandler, R.; Koo, Y.-M.

    1996-08-01

    Although x-ray micro-foci can be produced by a variety of diffractive methods, grazing incidence mirrors are the only route to an achromatic focus. In this paper we describe our efforts to produce elliptically shaped mirrors with the very high figure accuracy necessary for producing a micro-focus. The motivation for this work is provided by the need to produce achromatic foci for a range of applications ranging from tunable micro-focus x-ray photoelectron spectroscopy ({mu}-XPS) at soft x-ray energies to micro-focus white beam x-ray diffraction ({mu}-XRD) at hard x-ray energies. We describe the methodology of beam bending, a practical example of a system we have produced for {mu}-XRD, and results demonstrating the production of a surface with micro-radian figure accuracy.

  15. Deciphering Ni sequestration in soil ferromanganese nodules by combining x-ray fluorescence, absorption and diffraction at micrometer scales of resolution

    SciTech Connect (OSTI)

    Manceau, Alain; Tamura, Nobumichi; Marcus, Matthew A.; MacDowell, Alastair A.; Celestre, Richard S.; Sublett, Robert E.; Sposito, Garrison; Padmore, Howard A.

    2002-11-06

    X-ray microprobes are among the most important new analytical techniques to emerge from third generation synchrotron facilities. Here we show how X-ray fluorescence, diffraction, and absorption can be used in parallel to determine the structural form of trace elements in heterogeneous matrices at the micrometer-scale of resolution. Scanning X-ray microfluorescence (microSXRF) and microdiffraction (microSXRD) first are used to identify the host solid phase by mapping the distributions of elements and solid species, respectively. Micro-extended X-ray absorption fine structure (microEXAFS) spectroscopy is then used to determine the mechanism of trace element binding by the host phase at the molecular scale. To illustrate the complementary application of these three techniques, we studied how nickel is sequestered in soil ferromanganese nodules, an overwhelmingly complex natural matrix consisting of submicrometer to nanometer sized particles with varying structures and chemical composition s. We show that nickel substitutes for Mn3+ in the manganese layer of the MnO2-Al(OH)3 mixed-layer oxide lithiophorite. The affinity of Ni for lithiophorite was characteristic of micromodules sampled from soils across the U.S.A. and Europe. Since many natural and synthetic materials are heterogeneous at nanometer to micrometer scales, the synergistic use of microSXRF, microSXRD and microEXAFS is expected to have broad applications to earth and materials science.

  16. X-ray diffraction analysis of LiCu{sub 2}O{sub 2} crystals with additives of silver atoms

    SciTech Connect (OSTI)

    Sirotinkin, V. P. Bush, A. A.; Kamentsev, K. E.; Dau, H. S.; Yakovlev, K. A.; Tishchenko, E. A.

    2015-09-15

    Silver-containing LiCu{sub 2}O{sub 2} crystals up to 4 × 8 × 8 mm in size were grown by the crystallization of 80(1-x)CuO · 20{sub x}AgNO{sub 3} · 20Li{sub 2}CO{sub 3} (0 ≤ x ≤ 0.5) mixture melt. According to the X-ray spectral and Rietveld X-ray diffraction data, the maximum amount of silver incorporated in the LiCu{sub 2}O{sub 2} structure is about 4 at % relative to the copper content. It was established that silver atoms occupy statistically crystallographic positions of lithium atoms. The incorporation of silver atoms is accompanied by a noticeable increase in parameter c of the LiCu{sub 2}O{sub 2} rhombic unit cell, a slight increase in parameter a, and a slight decrease in parameter b.

  17. Magnetic properties of GdT2Zn20 (T = Fe, Co) investigated by x-ray diffraction and spectroscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    J. R. L. Mardegan; Fabbris, G.; Francoual, S.; Veiga, L. S. I.; Strempfer, J.; Haskel, D.; Ribeiro, R. A.; Avila, M. A.; Giles, C.

    2016-01-26

    In this study, we investigate the magnetic and electronic properties of the GdT2Zn20 (T=Fe and Co) compounds using x-ray resonant magnetic scattering (XRMS), x-ray absorption near-edge structure (XANES), and x-ray magnetic circular dichroism (XMCD). The XRMS measurements reveal that GdCo2Zn20 has a commensurate antiferromagnetic spin structure with a magnetic propagation vector →/τ = (12,12,12) below the Néel temperature (TN ~ 5.7 K). Only the Gd ions carry a magnetic moment forming an antiferromagnetic structure with magnetic representation Γ6. For the ferromagnetic GdFe2Zn20 compound, an extensive investigation was performed at low temperature and under magnetic field using XANES and XMCD. Amore » strong XMCD signal of about 12.5% and 9.7% is observed below the Curie temperature (TC ~ 85K) at the Gd L2 and L3 edges, respectively. In addition, a small magnetic signal of about 0.06% of the jump is recorded at the Zn K edge, suggesting that the Zn 4p states are spin polarized by the Gd 5d extended orbitals.« less

  18. Direct Observations of Austenite, Bainite and Martensite Formation During Arc Welding of 1045 Steel using Time Resolved X-Ray Diffraction

    SciTech Connect (OSTI)

    Elmer, J; Palmer, T; Babu, S; Zhang, W; DebRoy, T

    2004-02-17

    In-situ Time Resolved X-Ray Diffraction (TRXRD) experiments were performed during stationary gas tungsten arc (GTA) welding of AISI 1045 C-Mn steel. These synchrotron-based experiments tracked, in real time, phase transformations in the heat-affected zone of the weld under rapid heating and cooling conditions. The diffraction patterns were recorded at 100 ms intervals, and were later analyzed using diffraction peak profile analysis to determine the relative fraction of ferrite ({alpha}) and austenite ({gamma}) phases in each diffraction pattern. Lattice parameters and diffraction peak widths were also measured throughout the heating and cooling cycle of the weld, providing additional information about the phases that were formed. The experimental results were coupled with a thermofluid weld model to calculate the weld temperatures, allowing time-temperature transformation kinetics of the {alpha} {yields} {gamma} phase transformation to be evaluated. During heating, complete austenitization was observed in the heat affected zone of the weld and the kinetics of the {alpha} {yields} {gamma} phase transformation were modeled using a Johnson-Mehl-Avrami (JMA) approach. The results from the 1045 steel weld were compared to those of a 1005 low carbon steel from a previous study. Differences in austenitization rates of the two steels were attributed to differences in the base metal microstructures, particularly the relative amounts of pearlite and the extent of the allotriomorphic ferrite phase. During weld cooling, the austenite transformed to a mixture of bainite and martensite. In situ diffraction was able to distinguish between these two non-equilibrium phases based on differences in their lattice parameters and their transformation rates, resulting in the first real time x-ray diffraction observations of bainite and martensite formation made during welding.

  19. Crystallization and preliminary X-ray diffraction analysis of YidC, a membrane-protein chaperone and insertase from Bacillus halodurans

    SciTech Connect (OSTI)

    Kumazaki, Kaoru [The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); RIKEN, 2-1 Hirosawa, Wako-shi, Saitama 351-0198 (Japan); Tsukazaki, Tomoya, E-mail: ttsukaza@bs.naist.jp [Nara Institute of Science and Technology, 8916-5 Takayama-cho, Ikoma-shi, Nara 630-0192 (Japan); PRESTO, 4-1-8 Honcho, Kawaguchi, Saitama 332-0012 (Japan); Nishizawa, Tomohiro [The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); RIKEN, 2-1 Hirosawa, Wako-shi, Saitama 351-0198 (Japan); Tanaka, Yoshiki [Nara Institute of Science and Technology, 8916-5 Takayama-cho, Ikoma-shi, Nara 630-0192 (Japan); Kato, Hideaki E. [Stanford University, Stanford, CA 94305 (United States); Nakada-Nakura, Yoshiko [Kyoto University, Yoshidakonoe-cho, Sakyo-ku, Kyoto 606-8501 (Japan); Hirata, Kunio [RIKEN SPring-8 Center, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148 (Japan); Mori, Yoshihiro; Suga, Hiroaki [The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); Dohmae, Naoshi [RIKEN, 2-1 Hirosawa, Wako-shi, Saitama 351-0198 (Japan); Ishitani, Ryuichiro; Nureki, Osamu, E-mail: ttsukaza@bs.naist.jp [The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); RIKEN, 2-1 Hirosawa, Wako-shi, Saitama 351-0198 (Japan)

    2014-07-23

    YidC, a membrane-protein chaperone/insertase from B. halodurans, was expressed, purified and crystallized in the lipidic cubic phase. An X-ray diffraction data set was collected to 2.4 resolution. YidC, a member of the YidC/Oxa1/Alb3 family, inserts proteins into the membrane and facilitates membrane-protein folding in bacteria. YidC plays key roles in both Sec-mediated integration and Sec-independent insertion of membrane proteins. Here, Bacillus halodurans YidC2, which has five transmembrane helices conserved among the other family members, was identified as a target protein for structure determination by a fluorescent size-exclusion chromatography analysis. The protein was overexpressed, purified and crystallized in the lipidic cubic phase. The crystals diffracted X-rays to 2.4 resolution and belonged to space group P2{sub 1}, with unit-cell parameters a = 43.9, b = 60.6, c = 58.9 , ? = 100.3. The experimental phases were determined by the multiwavelength anomalous diffraction method using a mercury-derivatized crystal.

  20. The structural organization of N-methyl-2-pyrrolidone + water mixtures: A densitometry, x-ray diffraction, and molecular dynamics study

    SciTech Connect (OSTI)

    Usula, M.; Marincola, F. Cesare; Porcedda, S.; Mocci, F.; Gontrani, L.; Caminiti, R.

    2014-03-28

    A combined approach of molecular dynamics simulations, wide angle X-ray scattering experiments, and density measurements was employed to study the structural properties of N-methyl-2-pyrrolidone (NMP) + water mixtures over the whole concentration range. Remarkably, a very good agreement between computed and experimental densities and diffraction patterns was achieved, especially if the effect of the mixture composition on NMP charges is taken into account. Analysis of the intermolecular organization, as revealed by the radial and spatial distribution functions of relevant solvent atoms, nicely explained the density maximum observed experimentally.

  1. Temperature dependence of helium-implantation-induced lattice swelling in polycrystalline tungsten: X-ray micro-diffraction and Eigenstrain modelling

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    de Broglie, I.; Beck, C. E.; Liu, W.; Hofmann, Felix

    2015-05-30

    Using synchrotron X-ray micro-diffraction and Eigenstrain analysis the distribution of lattice swelling near grain boundaries in helium-implanted polycrystalline tungsten is quantified. Samples heat-treated at up to 1473 K after implantation show less uniform lattice swelling that varies significantly from grain to grain compared to as-implanted samples. An increase in lattice swelling is found in the vicinity of some grain boundaries, even at depths beyond the implanted layer. As a result, these findings are discussed in terms of the evolution of helium-ion-implantation-induced defects.

  2. High-Pressure Raman Spectroscopy and X-ray Diffraction Studies of a Terpolymer of Tetrafluoroethylene-Hexafluoropropylene-Vinylidene Fluoride: THV 500

    SciTech Connect (OSTI)

    Emmons, E.D.; Velisavljevic, N.; Schoonover, J.R.; Dattelbaum, D.M.

    2008-04-02

    High-pressure Raman spectroscopy and X-ray diffraction of THV 500, a terpolymer of tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride, were performed using diamond anvil cells (DAC). Changes in the interatomic spacing as well as shifts of several of the vibrational bands as a function of pressure were measured up to {approx}10 GPa. The changes in interatomic spacing and shifts of the vibrational bands are compared to those of polytetrafluoroethylene, showing the effects of copolymerization and reduced crystallinity. The high-pressure behavior of polymers is a relatively unexplored field but is becoming increasingly important due to applications where polymers experience extreme conditions.

  3. High-Pressure Synchtron Radiation X-Ray Diffraction Studies of Pentaerythritol Tetranitrate C(CH[subscript 2]ONO[subscript 2 ])[subscript 4

    SciTech Connect (OSTI)

    Lipinska-Kalita, K.E.; Pravica, M.; Nicol, M.

    2006-02-02

    A high-pressure x-ray diffraction study of nanocrystalline pentaerythritol tetranitrate, C(CH{sub 2}ONO{sub 2}){sub 4}, (PETN), has been performed in a diamond-anvil cell at ambient temperature using synchrotron radiation. Pressure-induced alterations in the profiles of the diffraction lines, including their positions, widths and intensities were followed up to 30 GPa in a compressino cycle. The spectral changes in the diffraction patterns at low pressures indicated continuous densification of the tetragonal structure (space group P{bar 4}2{sub 1}c). The diffraction patterns confirmed that PETN compressed from ambient pressure to 7.4 GPa by 17%. At 8.2 GPa and above, several new diffraction lines appeared in the patterns. These lines suggest that the lattice undergoes an incomplete stress-induced structural transformation from the tetragonal to an orthorhombic structure (most probably space group P2{sub 1}22{sub 1}). The mixture of both structures appeared to persist to 30 GPa. The progressive broadening of the diffraction lines as the pressure increased beyond 10 GPa is attributed to the combined diffraction lines of a mixture of two coexisting PETN phases and inhomogeneous pressure distribution within the sample.

  4. Single-particle structure determination by correlations of snapshot X-ray diffraction patterns (CXIDB ID 20)

    DOE Data Explorer [Office of Scientific and Technical Information (OSTI)]

    Starodub, D.

    2013-03-25

    This deposition includes the diffraction images generated by the paired polystyrene spheres in random orientations. These images were used to determine and phase the single particle diffraction volume from their autocorrelation functions.

  5. Characterization of morphology and hydration products of high-volume fly ash paste by monochromatic scanning x-ray micro-diffraction (?-SXRD)

    SciTech Connect (OSTI)

    Bae, Sungchul; Meral, Cagla; Oh, Jae-eun; Moon, Juhyuk; Kunz, Martin; Monteiro, Paulo J.M.

    2014-05-01

    The present study focuses on identification and micro-structural characterization of the hydration products formed in high-volume fly ash (HVFA)/portland cement (PC) systems using monochromatic scanning x-ray micro-diffraction (?-SXRD) and SEM-EDS. Pastes with up to 80% fly ash replacement were studied. Phase maps for HVFA samples using ?-SXRD patterns prove that ?-SXRD is an effective method to identify and visualize the distribution of phases in the matrix. ?-SXRD and SEM-EDS analysis shows that the C-S-H formed in HVFA system containing 50% or more of fly ash has a similar structure as C-S-H(I) with comparatively lower Ca/Si ratio than the one produced in PC system. Moreover, coexistence of C-S-H(I) and strtlingite is observed in the system containing 80% of fly ash, confirming that the amount of alumina and silicate phases provided by the fly ash is a major factor for the formation of C-S-H(I) and strtlingite in HVFA system. - Highlights: High-volume fly ash (HVFA) paste was studied by scanning x-ray micro-diffraction. Coexistence of C-S-H(I) and strtlingite in the HVFA system is clearly shown. The distribution of minor phases in the HVFA system is shown. Differences between inner and outer products of fly ash are observed by SEM-EDS.

  6. Direct Observation of Phase Transformations in Austenitic Stainless Steel Welds Using In-situ Spatially Resolved and Time-resolved X-ray Diffraction

    SciTech Connect (OSTI)

    Elmer, J.; Wong, J.; Ressler, T.

    1999-09-23

    Spatially resolved x-ray diffraction (SRXRD) and time resolved x-ray diffraction (TRXRD) were used to investigate real time solid state phase transformations and solidification in AISI type 304 stainless steel gas tungsten arc (GTA) welds. These experiments were conducted at Stanford Synchrotron Radiation Laboratory (SSRL) using a high flux beam line. Spatially resolved observations of {gamma} {leftrightarrow} {delta} solid state phase transformations were performed in the heat affected zone (HAZ) of moving welds and time-resolved observations of the solidification sequence were performed in the fusion zone (FZ) of stationary welds after the arc had been terminated. Results of the moving weld experiments showed that the kinetics of the {gamma}{yields}{delta} phase transformation on heating in the HAZ were sufficiently rapid to transform a narrow region surrounding the liquid weld pool to the {delta} ferrite phase. Results of the stationary weld experiments showed, for the first time, that solidification can occur directly to the {delta} ferrite phase, which persisted as a single phase for 0.5s. Upon solidification to {delta}, the {delta} {yields} {gamma} phase transformation followed and completed in 0.2s as the weld cooled further to room temperature.

  7. Characterization of room temperature recrystallization kinetics in electroplated copper thin films with concurrent x-ray diffraction and electrical resistivity measurements

    SciTech Connect (OSTI)

    Treger, Mikhail; Noyan, I. C.; Witt, Christian; Cabral, Cyril; Murray, Conal; Jordan-Sweet, Jean; Rosenberg, Robert; Eisenbraun, Eric

    2013-06-07

    Concurrent in-situ four-point probe resistivity and high resolution synchrotron x-ray diffraction measurements were used to characterize room temperature recrystallization in electroplated Cu thin films. The x-ray data were used to obtain the variation with time of the integrated intensities and the peak-breadth from the Cu 111 and 200 reflections of the transforming grains. The variation of the integrated intensity and resistivity data with time was analyzed using the Johnson-Mehl-Avrami-Kolmogorov (JMAK) model. For both 111-textured and non-textured electroplated Cu films, four-point probe resistivity measurements yielded shorter transformation times than the values obtained from the integrated intensities of the corresponding Cu 111 reflections. In addition, the JMAK exponents fitted to the resistivity data were significantly smaller. These discrepancies could be explained by considering the different material volumes from which resistivity and diffraction signals originated, and the physical processes which linked these signals to the changes in the evolving microstructure. Based on these issues, calibration of the resistivity analysis with direct structural characterization techniques is recommended.

  8. Thermal strains in focusing channels of the stations for X-ray diffraction analysis in the Sibir-2 storage ring

    SciTech Connect (OSTI)

    Kheiker, D. M.; Konoplev, E. E.; Molodenskii, D. S.; Shishkov, V. A.; Dorovatovskii, P. V.

    2010-09-15

    The thermal load caused by the absorption of synchrotron radiation in X-ray optical elements of the Belok and RSA stations leads to optics elements heating and induces strains upon simultaneous cooling. The heating of the cooled first crystal in the double-crystal monochromator causes its bending and increases the reflected beam divergence, which, in turn, results in the monochromatic beam intensity loss [1]. Numerical simulation makes it possible to more accurately determine the strains, choose the optimal monochromator design, estimate the vertical sizes of the focal spot and wavelength resolution in the focusing channel, correctly design the system for cooling the mirror at the channel input, and choose a design providing the minimum temperature of the beam-limiting slit knives.

  9. Cloning, expression, purification, crystallization and preliminary X-ray diffraction analysis of human ARH3, the first eukaryotic protein-ADP-ribosylhydrolase

    SciTech Connect (OSTI)

    Kernstock, Stefan; Koch-Nolte, Friedrich; Mueller-Dieckmann, Jochen; Weiss, Manfred S.; Mueller-Dieckmann, Christoph

    2006-03-01

    Human ADP-ribosylhydrolase 3 (ARH3), which has been identified as an ARH by a sequence-similarity search and which cleaves the glycosidic bond of ADP-ribose attached to a protein, has been cloned, expressed, purified and crystallized in two different space groups. ADP-ribosylhydrolases catalyze the release of ADP-ribose from ADP-ribosylated proteins via hydrolysis of the glycosidic bond between ADP-ribose and a specific amino-acid residue in a target protein. Human ADP-ribosylhydrolase 3, consisting of 347 amino-acid residues, has been cloned and heterologously expressed in Escherichia coli, purified and crystallized in two different space groups. Preliminary X-ray diffraction studies yielded excellent diffraction data to a resolution of 1.6 Å.

  10. X-ray shearing interferometer

    DOE Patents [OSTI]

    Koch, Jeffrey A.

    2003-07-08

    An x-ray interferometer for analyzing high density plasmas and optically opaque materials includes a point-like x-ray source for providing a broadband x-ray source. The x-rays are directed through a target material and then are reflected by a high-quality ellipsoidally-bent imaging crystal to a diffraction grating disposed at 1.times. magnification. A spherically-bent imaging crystal is employed when the x-rays that are incident on the crystal surface are normal to that surface. The diffraction grating produces multiple beams which interfere with one another to produce an interference pattern which contains information about the target. A detector is disposed at the position of the image of the target produced by the interfering beams.