Synchrotron powder diffraction on Aztec blue pigments

NASA Astrophysics Data System (ADS)

Sánchez Del Río, M.; Gutiérrez-León, A.; Castro, G. R.; Rubio-Zuazo, J.; Solís, C.; Sánchez-Hernández, R.; Robles-Camacho, J.; Rojas-Gaytán, J.

2008-01-01

Some samples of raw blue pigments coming from an archaeological rescue mission in downtown Mexico City have been characterized using different techniques. The samples, some recovered as a part of a ritual offering, could be assigned to the late Aztec period (XVth century). The striking characteristic of these samples is that they seem to be raw pigments prior to any use in artworks, and it was possible to collect a few μg of pigment after manual grain selection under a microscopy monitoring. All pigments are made of indigo, an organic colorant locally known as añil or xiuhquilitl. The colorant is always found in combination with an inorganic matrix, studied by powder diffraction. In one case the mineral base is palygorskite, a rare clay mineral featuring micro-channels in its structure, well known as the main ingredient of the Maya blue pigment. However, other samples present the minerals sepiolite (a clay mineral of the palygorskite family) and calcite. Another sample contains barite, a mineral never reported in prehispanic paints. We present the results of characterization using high resolution powder diffraction recorded at the European Synchrotron Radiation Facility (BM25A, SpLine beamline) complemented with other techniques. All of them gave consistent results on the composition. A chemical test on resistance to acids was done, showing a high resistance for the palygorskite and eventually sepiolite compounds, in good agreement with the excellent resistance of the Maya blue.

The new HMI beamline MAGS: an instrument for hard X-ray diffraction at BESSY.

PubMed

Dudzik, Esther; Feyerherm, Ralf; Diete, Wolfgang; Signorato, Riccardo; Zilkens, Christopher

2006-11-01

The Hahn-Meitner-Institute Berlin is operating the new hard X-ray diffraction beamline MAGS at the Berlin synchrotron radiation source BESSY. The beamline is intended to complement the existing neutron instrumentation at the Berlin Neutron Scattering Centre. The new beamline uses a 7 T multipole wiggler to produce photon fluxes in the 10(11)-10(12) photons s(-1) (100 mA)(-1) (0.1% bandwidth)(-1) range at energies from 4 to 30 keV at the experiment. It has active bendable optics to provide flexible horizontal and vertical focusing and to compensate the large heat load from the wiggler source. The experimental end-station consists of a six-circle Huber diffractometer which can be used with an additional (polarization) analyser and different sample environments. The beamline is intended for single-crystal diffraction and resonant magnetic scattering experiments for the study of ordering phenomena, phase transitions and materials science.

Advanced Spectral Analysis Program (ASAP) for High-Pressure X-ray Diffraction

NASA Astrophysics Data System (ADS)

Montgomery, Jeffrey

A program for analyzing large powder diffraction data sets has been developed. This tool enables the user to fit any type of crystal structure by indexing peaks in multiple files simultaneously by manually selecting them from a 2D plot of peak positions. The program has tools for automatic peak fitting and pressure determination using various equations of state. The interface is useful for correlating information from various types of spectral data, and so tools have been added for analyzing common fluorescence markers such as ruby, strontium tetraborate, and diamond. The program operation is demonstrated by the analysis of high-pressure powder x-ray diffraction data taken on a sample of vanadium metal at the Advanced Photon Source 16-BMD beamline. Samples were compressed in three runs to a pressure of 70 GPa in an attempt to measure the phase transition from bcc to orthorhombic in hydrostatic and non-hydrostatic conditions. Using ASAP to analyze this data provides a fast and accurate tool for observation of such a subtle transition, which is characterized primarily by a narrow splitting of the bcc 110 and 112 peaks. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

Coherent X-ray beam metrology using 2D high-resolution Fresnel-diffraction analysis.

PubMed

Ruiz-Lopez, M; Faenov, A; Pikuz, T; Ozaki, N; Mitrofanov, A; Albertazzi, B; Hartley, N; Matsuoka, T; Ochante, Y; Tange, Y; Yabuuchi, T; Habara, T; Tanaka, K A; Inubushi, Y; Yabashi, M; Nishikino, M; Kawachi, T; Pikuz, S; Ishikawa, T; Kodama, R; Bleiner, D

2017-01-01

Direct metrology of coherent short-wavelength beamlines is important for obtaining operational beam characteristics at the experimental site. However, since beam-time limitation imposes fast metrology procedures, a multi-parametric metrology from as low as a single shot is desirable. Here a two-dimensional (2D) procedure based on high-resolution Fresnel diffraction analysis is discussed and applied, which allowed an efficient and detailed beamline characterization at the SACLA XFEL. So far, the potential of Fresnel diffraction for beamline metrology has not been fully exploited because its high-frequency fringes could be only partly resolved with ordinary pixel-limited detectors. Using the high-spatial-frequency imaging capability of an irradiated LiF crystal, 2D information of the coherence degree, beam divergence and beam quality factor M 2 were retrieved from simple diffraction patterns. The developed beam metrology was validated with a laboratory reference laser, and then successfully applied at a beamline facility, in agreement with the source specifications.

The Protein Micro-Crystallography Beamlines for Targeted Protein Research Program

NASA Astrophysics Data System (ADS)

Hirata, Kunio; Yamamoto, Masaki; Matsugaki, Naohiro; Wakatsuki, Soichi

In order to collect proper diffraction data from outstanding micro-crystals, a brand-new data collection system should be designed to provide high signal-to noise ratio in diffraction images. SPring-8 and KEK-PF are currently developing two micro-beam beamlines for Targeted Proteins Research Program by MEXT of Japan. The program aims to reveal the structure and function of proteins that are difficult to solve but have great importance in both academic research and industrial application. At SPring-8, a new 1-micron beam beamline for protein micro-crystallography, RIKEN Targeted Proteins Beamline (BL32XU), is developed. At KEK-PF a new low energy micro-beam beamline, BL-1A, is dedicated for SAD micro-crystallography. The two beamlines will start operation in the end of 2010. The present status of the research and development for protein micro-crystallography will be presented.

Structure and thermal expansion of Ca9Gd(VO4)7: A combined powder-diffraction and dilatometric study of a Czochralski-grown crystal

NASA Astrophysics Data System (ADS)

Paszkowicz, Wojciech; Shekhovtsov, Alexei; Kosmyna, Miron; Loiko, Pavel; Vilejshikova, Elena; Minikayev, Roman; Romanowski, Przemysław; Wierzchowski, Wojciech; Wieteska, Krzysztof; Paulmann, Carsten; Bryleva, Ekaterina; Belikov, Konstantin; Fitch, Andrew

2017-11-01

Materials of the Ca9RE(VO4)7 (CRVO) formula (RE = rare earth) and whitlockite-related structures are considered for applications in optoelectronics, e.g., in white-light emitting diodes and lasers. In the CRVO structure, the RE atoms are known to share the site occupation with Ca atoms at two or three among four Ca sites, with partial occupancy values depending on the choice of the RE atom. In this work, the structure and quality of a Czochralski-grown crystal of this family, Ca9Gd(VO4)7 (CGVO), are studied using X-ray diffraction methods. The room-temperature structure is refined using the powder diffraction data collected at a high-resolution synchrotron beamline ID22 (ESRF, Grenoble); for comparison purposes, a laboratory diffraction pattern was collected and analyzed, as well. The site occupancies are discussed on the basis of comparison with literature data of isostructural synthetic crystals of the CRVO series. The results confirm the previously reported site-occupation scheme and indicate a tendency of the CGVO compound to adopt a Gd-deficient composition. Moreover, the thermal expansion coefficient is determined for CGVO as a function of temperature in the 302-1023 K range using laboratory diffraction data. Additionally, for CGVO and six other single crystals of the same family, thermal expansion is studied in the 298-473 K range, using the dilatometric data. The magnitude and anisotropy of thermal expansion, being of importance for laser applications, are discussed for these materials.

PF-AR NW14, a new time-resolved diffraction/scattering beamline

NASA Astrophysics Data System (ADS)

Nozawa, Shunsuke; Adachi, Shin-ichi; Tazaki, Ryoko; Takahashi, Jun-ichi; Itatani, Jiro; Daimon, Masahiro; Mori, Takeharu; Sawa, Hiroshi; Kawata, Hiroshi; Koshihara, Shin-ya

2005-01-01

NW14 is a new insertion device beamline at the Photon Factory Advanced Ring (PF-AR), which is a unique ring with full-time single-bunched operation, aiming for timeresolved x-ray diffraction/scattering and XAFS experiments. The primary scientific goal of this beamline is to observe the ultrafast dynamics of condensed matter systems such as organic and inorganic crystals, biological systems and liquids triggered by optical pulses. With the large photon fluxes derived from the undulator, it should become possible to take a snapshoot an atomic-scale image of the electron density distribution. By combining a series of images it is possible to produce a movie of the photo-induced dynamics with 50-ps resolution. The construction of the beamline is being funded by the ERATO Koshihara Non-equilibrium Dynamics Project of the Japan Science and Technology Agency (JST), and the beamline will be operational from autumn 2005.

Protein crystallography beamline BL2S1 at the Aichi synchrotron

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

Watanabe, Nobuhisa; Nagae, Takayuki; Yamada, Yusuke

The protein crystallography beamline BL2S1, constructed at one of the 5 T superconducting bending-magnet ports of the Aichi synchrotron, is available to users associated with academic and industrial organizations. The beamline is mainly intended for use in X-ray diffraction measurements of single-crystals of macromolecules such as proteins and nucleic acids. Diffraction measurements for crystals of other materials are also possible, such as inorganic and organic compounds. BL2S1 covers the energy range 7–17 keV (1.8–0.7 Å) with an asymmetric-cut curved single-crystal monochromator [Ge(111) or Ge(220)], and a platinum-coated Si mirror is used for vertical focusing and as a higher-order cutoff filter.more » The beamline is equipped with a single-axis goniometer, a CCD detector, and an open-flow cryogenic sample cooler. Lastly, high-pressure protein crystallography with a diamond anvil cell can also be performed using this beamline.« less

Protein crystallography beamline BL2S1 at the Aichi synchrotron.

PubMed

Watanabe, Nobuhisa; Nagae, Takayuki; Yamada, Yusuke; Tomita, Ayana; Matsugaki, Naohiro; Tabuchi, Masao

2017-01-01

The protein crystallography beamline BL2S1, constructed at one of the 5 T superconducting bending-magnet ports of the Aichi synchrotron, is available to users associated with academic and industrial organizations. The beamline is mainly intended for use in X-ray diffraction measurements of single-crystals of macromolecules such as proteins and nucleic acids. Diffraction measurements for crystals of other materials are also possible, such as inorganic and organic compounds. BL2S1 covers the energy range 7-17 keV (1.8-0.7 Å) with an asymmetric-cut curved single-crystal monochromator [Ge(111) or Ge(220)], and a platinum-coated Si mirror is used for vertical focusing and as a higher-order cutoff filter. The beamline is equipped with a single-axis goniometer, a CCD detector, and an open-flow cryogenic sample cooler. High-pressure protein crystallography with a diamond anvil cell can also be performed using this beamline.

The GKSS beamlines at PETRA III and DORIS III

NASA Astrophysics Data System (ADS)

Haibel, A.; Beckmann, F.; Dose, T.; Herzen, J.; Utcke, S.; Lippmann, T.; Schell, N.; Schreyer, A.

2008-08-01

Due to the high brilliance of the new storage ring PETRA III at DESY in Hamburg, the low emittance of 1 nmrad and the high fraction of coherent photons also in the hard X-ray range extremely intense and sharply focused X-ray light will be provided. These advantages of the beam fulfill excellently the qualifications for the planned Imaging BeamLine IBL and the High Energy Materials Science Beamline (HEMS) at PETRA III, i.e. for absorption tomography, phase enhanced and phase contrast experiments, for diffraction, for nano focusing, for nano tomography, and for high speed or in-situ experiments with highest spatial resolution. The existing HARWI II beamline at the DORIS III storage ring at DESY completes the GKSS beamline concept with setups for high energy tomography (16-150 keV) and diffraction (16-250 keV), characterized by a large field of view and an excellent absorption contrast with spatial resolutions down to 2 μm.

HYBRID Simulations of Diffraction-Limited Focusing with Kirkpatrick-Baez Mirrors for a Next-Generation In Situ Hard X-ray Nanoprobe

NASA Astrophysics Data System (ADS)

Maser, Jörg; Shi, Xianbo; Reininger, Ruben; Lai, Barry; Vogt, Stefan

2016-12-01

Next-generation hard X-ray nanoprobe beamlines such as the In Situ Nanoprobe (ISN) beamline being planned at the Advanced Photon Source aim at providing very high spatial resolution while also enabling very high focused flux, to study complex materials and devices using fast, multidimensional imaging across many length scales. The ISN will use diffractive optics to focus X-rays with a bandpass of Δ E/ E = 10-4 into a focal spot of 20 nm or below. Reflective optics in Kirkpatrick-Baez geometry will be used to focus X-rays with a bandpass as large as Δ E/ E = 10-2 into a focal spot of 50 nm. Diffraction-limited focusing with reflective optics is achieved by spatial filtering and use of a very long, vertically focusing mirror. To quantify the performance of the ISN beamline, we have simulated the propagation of both partially and fully coherent wavefronts from the undulator source, through the ISN beamline and into the mirror-based focal spot. Simulations were carried out using the recently developed software " HYBRID."

PSICHE: a new beamline dedicated to X-ray diffraction and tomography at high pressure at synchrotron SOLEIL

NASA Astrophysics Data System (ADS)

Guignot, N.; Itié, J.; Zerbino, P.; Delmotte, A.; Moreno, T.

2013-12-01

The PSICHE beamline (for 'Pressure, Structure and Imaging by Contrast at High Energy') is a new facility opened for high pressure experiments at synchrotron SOLEIL (St-Aubin, France). With its source, optics, detectors and 3 experimental stations, it can handle a large variety of experimental setups. High energy photons are produced with an in-vacuum wiggler. The white beam obtained, with photons energy ranging continuously from 15 to 80 keV (from a 2.75 GeV machine), is used on the first experimental station for energy dispersive X-ray diffraction (EDX) measurements using different pressure cells. The main setup is a 1200 tons load capacity multi-anvil press featuring a (100) DIA compression module with a 15° horizontal aperture, allowing measurements up to 30° in 2theta by rotating the press. Other setups are a Paris-Edinburgh (PE) large volume press and diamond anvil cells (DACs). On the detection side we have a rotating Ge detector, based on the CAESAR design described by Wang et al. (2004) (combination of EDX and angular dispersive X-ray diffraction, ADX). One of the difficulties when building such setups is the rotation mechanism which cannot be physically attached to the rotation axis, potentially leading to large circle of confusions on the horizontal position of this axis. Thanks to translation corrections done at each angle step, the circle of confusion is minimized to 3x6 μm2 along the 35° travel, making possible measurements on very small objects. Combining EDX and ADX has a lot of advantages and we will present our first results obtained using this setup. The PSICHE focusing optics and monochromator are also used to focus monochromatic beams (up to 52 keV) on 2 different experimental stations. The first focal point at 31 m gives a beam size of 100x50 μm2 (HxV) and is useful for low pressure experiments and experiments done with the PE press associated with Soller slits. A PerkinElmer flatpanel detector can be precisely scanned in 3 directions, making ADX measurements at the highest possible resolution on this beamline. This station will also be used for diffraction tomography experiments. The second focal point at 37.6 m is located behind KB mirrors on the third experimental station. 10x10 μm2 beam sizes (full width) are expected. This station will be used for DAC experiments, with or without our future laser heating setup. Finally, parallel beams can be produced with sizes up to 15x5 mm2 (HxV) for tomography experiments, in pink (filtered white) beam or monochromatic beam. We plan to use rotating anvils presses such as the rotoPEc (J. Philippe et al., 2013) to take full advantage of this beam mode, but it can be opened to other techniques. The PSICHE beamline is opened for users since July 2013. Some stations are not available yet, and will be opened through 2014 and 2015. References X. Dong et al., Ray tracing application in hard x-ray optical development: Soleil first wiggler beamline (PSICHÉ) case" (2011), Proc. SPIE 8141, 814113 Y. Wang et al., A new technique for angle-dispersive powder diffraction using an energy-dispersive setup and synchrotron radiation (2004), J. Appl. Cryst. 37, 947-956 J. Philippe, Y. Le Godec, F. Bergame et M. Morand, Patent INPI 11 62335 (2013)

Single-drop optimization of protein crystallization.

PubMed

Meyer, Arne; Dierks, Karsten; Hilterhaus, Dierk; Klupsch, Thomas; Mühlig, Peter; Kleesiek, Jens; Schöpflin, Robert; Einspahr, Howard; Hilgenfeld, Rolf; Betzel, Christian

2012-08-01

A completely new crystal-growth device has been developed that permits charting a course across the phase diagram to produce crystalline samples optimized for diffraction experiments. The utility of the device is demonstrated for the production of crystals for the traditional X-ray diffraction data-collection experiment, of microcrystals optimal for data-collection experiments at a modern microbeam insertion-device synchrotron beamline and of nanocrystals required for data collection on an X-ray laser beamline.

High-energy cryo x-ray nano-imaging at the ID16A beamline of ESRF

NASA Astrophysics Data System (ADS)

da Silva, Julio C.; Pacureanu, Alexandra; Yang, Yang; Fus, Florin; Hubert, Maxime; Bloch, Leonid; Salome, Murielle; Bohic, Sylvain; Cloetens, Peter

2017-09-01

The ID16A beamline at ESRF offers unique capabilities for X-ray nano-imaging, and currently produces the worlds brightest high energy diffraction-limited nanofocus. Such a nanoprobe was designed for quantitative characterization of the morphology and the elemental composition of specimens at both room and cryogenic temperatures. Billions of photons per second can be delivered in a diffraction-limited focus spot size down to 13 nm. Coherent X-ray imaging techniques, as magnified holographic-tomography and ptychographic-tomography, are implemented as well as X-ray fluorescence nanoscopy. We will show the latest developments in coherent and spectroscopic X-ray nanoimaging implemented at the ID16A beamline

Shining a light on planetary processes using synchrotron techniques

NASA Astrophysics Data System (ADS)

Brand, H. E. A.; Kimpton, J. A.

2017-12-01

The Australian Synchrotron is a world-class national research facility that uses accelerator technology to produce X-rays and infrared for research. It is available for researchers from all institutions and disciplines. This contribution is intended to inform the community of the current capabilities at the facility using examples drawn from planetary research across the beamlines. Examples will include: formation of jarosite minerals with a view to Mars; studies of Micrometeorites; and large volume CT imaging of geological samples. A suite of new beamlines has been proposed for the growth of the facility and one of these, ADS, the Advanced Diffraction and Scattering beamline, is intended to be a high energy X-ray diffraction beamline capable of reaching extreme conditions and carrying out challenging in situ experiments. There is an opportunity to develop complex new sample environments which could be of relevance to shock metamorphic processes and this will form part of the discussion.

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

An electrochemical cell with sapphire windows for operando synchrotron X-ray powder diffraction and spectroscopy studies of high-power and high-voltage electrodes for metal-ion batteries.

PubMed

Drozhzhin, Oleg A; Tereshchenko, Ivan V; Emerich, Hermann; Antipov, Evgeny V; Abakumov, Artem M; Chernyshov, Dmitry

2018-03-01

A new multi-purpose operando electrochemical cell was designed, constructed and tested on the Swiss-Norwegian Beamlines BM01 and BM31 at the European Synchrotron Radiation Facility. Single-crystal sapphire X-ray windows provide a good signal-to-noise ratio, excellent electrochemical contact because of the constant pressure between the electrodes, and perfect electrochemical stability at high potentials due to the inert and non-conductive nature of sapphire. Examination of the phase transformations in the Li 1-x Fe 0.5 Mn 0.5 PO 4 positive electrode (cathode) material at C/2 and 10C charge and discharge rates, and a study of the valence state of the Ni cations in the Li 1-x Ni 0.5 Mn 1.5 O 4 cathode material for Li-ion batteries, revealed the applicability of this novel cell design to diffraction and spectroscopic investigations of high-power/high-voltage electrodes for metal-ion batteries.

Structure of the cyanobactin oxidase ThcOx from Cyanothece sp. PCC 7425, the first structure to be solved at Diamond Light Source beamline I23 by means of S-SAD.

PubMed

Bent, Andrew F; Mann, Greg; Houssen, Wael E; Mykhaylyk, Vitaliy; Duman, Ramona; Thomas, Louise; Jaspars, Marcel; Wagner, Armin; Naismith, James H

2016-11-01

Determination of protein crystal structures requires that the phases are derived independently of the observed measurement of diffraction intensities. Many techniques have been developed to obtain phases, including heavy-atom substitution, molecular replacement and substitution during protein expression of the amino acid methionine with selenomethionine. Although the use of selenium-containing methionine has transformed the experimental determination of phases it is not always possible, either because the variant protein cannot be produced or does not crystallize. Phasing of structures by measuring the anomalous diffraction from S atoms could in theory be almost universal since almost all proteins contain methionine or cysteine. Indeed, many structures have been solved by the so-called native sulfur single-wavelength anomalous diffraction (S-SAD) phasing method. However, the anomalous effect is weak at the wavelengths where data are normally recorded (between 1 and 2 Å) and this limits the potential of this method to well diffracting crystals. Longer wavelengths increase the strength of the anomalous signal but at the cost of increasing air absorption and scatter, which degrade the precision of the anomalous measurement, consequently hindering phase determination. A new instrument, the long-wavelength beamline I23 at Diamond Light Source, was designed to work at significantly longer wavelengths compared with standard synchrotron beamlines in order to open up the native S-SAD method to projects of increasing complexity. Here, the first novel structure, that of the oxidase domain involved in the production of the natural product patellamide, solved on this beamline is reported using data collected to a resolution of 3.15 Å at a wavelength of 3.1 Å. The oxidase is an example of a protein that does not crystallize as the selenium variant and for which no suitable homology model for molecular replacement was available. Initial attempts collecting anomalous diffraction data for native sulfur phasing on a standard macromolecular crystallography beamline using a wavelength of 1.77 Å did not yield a structure. The new beamline thus has the potential to facilitate structure determination by native S-SAD phasing for what would previously have been regarded as very challenging cases with modestly diffracting crystals and low sulfur content.

Coherent Bragg nanodiffraction at the hard X-ray Nanoprobe beamline.

PubMed

Hruszkewycz, S O; Holt, M V; Maser, J; Murray, C E; Highland, M J; Folkman, C M; Fuoss, P H

2014-03-06

Bragg coherent diffraction with nanofocused hard X-ray beams provides unique opportunities for quantitative in situ studies of crystalline structure in nanoscale regions of complex materials and devices by a variety of diffraction-based techniques. In the case of coherent diffraction imaging, a major experimental challenge in using nanoscale coherent beams is maintaining a constant scattering volume such that coherent fringe visibility is maximized and maintained over the course of an exposure lasting several seconds. Here, we present coherent Bragg diffraction patterns measured from different nanostructured thin films at the Sector 26 Nanoprobe beamline at the Advanced Photon Source and demonstrate that with nanoscale positional control, coherent diffraction patterns can be measured with source-limited fringe visibilities more than 50% suitable for imaging by coherent Bragg ptychography techniques.

Coherent Bragg nanodiffraction at the hard X-ray Nanoprobe beamline

PubMed Central

Hruszkewycz, S. O.; Holt, M. V.; Maser, J.; Murray, C. E.; Highland, M. J.; Folkman, C. M.; Fuoss, P. H.

2014-01-01

Bragg coherent diffraction with nanofocused hard X-ray beams provides unique opportunities for quantitative in situ studies of crystalline structure in nanoscale regions of complex materials and devices by a variety of diffraction-based techniques. In the case of coherent diffraction imaging, a major experimental challenge in using nanoscale coherent beams is maintaining a constant scattering volume such that coherent fringe visibility is maximized and maintained over the course of an exposure lasting several seconds. Here, we present coherent Bragg diffraction patterns measured from different nanostructured thin films at the Sector 26 Nanoprobe beamline at the Advanced Photon Source and demonstrate that with nanoscale positional control, coherent diffraction patterns can be measured with source-limited fringe visibilities more than 50% suitable for imaging by coherent Bragg ptychography techniques. PMID:24470418

HYBRID simulations of diffraction-limited focusing with Kirkpatrick-Baez mirrors for a next-generation In Situ hard X-ray nanoprobe

DOE PAGES

Maser, Jorg; Shi, Xianbo; Reininger, Ruben; ...

2016-02-22

Next-generation hard X-ray nanoprobe beamlines such as the In Situ Nanoprobe (ISN) beamline being planned at the Advanced Photon Source aim at providing very high spatial resolution while also enabling very high focused flux, to study complex materials and devices using fast, multidimensional imaging across many length scales. The ISN will use diffractive optics to focus X-rays with a bandpass of ΔE/E = 10 –4 into a focal spot of 20 nm or below. Reflective optics in Kirkpatrick-Baez geometry will be used to focus X-rays with a bandpass as large as ΔE/E = 10 –2 into a focal spot ofmore » 50 nm. Diffraction-limited focusing with reflective optics is achieved by spatial filtering and use of a very long, vertically focusing mirror. Furthermore, to quantify the performance of the ISN beamline, we have simulated the propagation of both partially and fully coherent wavefronts from the undulator source, through the ISN beamline and into the mirror-based focal spot. Simulations were carried out using the recently developed software “HYBRID.”« less

Status of the Nanoscopium Scanning Hard X-ray Nanoprobe Beamline of Synchrotron Soleil

NASA Astrophysics Data System (ADS)

Somogyi, A.; Kewish, C. M.; Ribbens, M.; Moreno, T.; Polack, F.; Baranton, G.; Desjardins, K.; Samama, J. P.

2013-10-01

The Nanoscopium 155 m-long scanning hard X-ray nanoprobe beamline of Synchrotron Soleil (St Aubin, France) is dedicated to quantitative multi-modal 2D/3D imaging. The beamline aims to reach down to 30 nm spatial resolution in the 5-20 keV energy range. Two experimental stations working in consecutive operation mode will be dedicated to coherent diffractive imaging and scanning X-ray nanoprobe techniques. The beamline is in the construction phase, the first user experiments are expected in 2014. The main characteristics of the beamline and an overview of its status are given in this paper.

Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging

PubMed Central

Warren, Anna J.; Armour, Wes; Axford, Danny; Basham, Mark; Connolley, Thomas; Hall, David R.; Horrell, Sam; McAuley, Katherine E.; Mykhaylyk, Vitaliy; Wagner, Armin; Evans, Gwyndaf

2013-01-01

The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required. PMID:23793151

Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging.

PubMed

Warren, Anna J; Armour, Wes; Axford, Danny; Basham, Mark; Connolley, Thomas; Hall, David R; Horrell, Sam; McAuley, Katherine E; Mykhaylyk, Vitaliy; Wagner, Armin; Evans, Gwyndaf

2013-07-01

The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required.

Micro- and nano-imaging at the diamond beamline I13L-imaging and coherence

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

Rau, C., E-mail: Christoph.rau@diamond.ac.uk; University of Manchester, School of Materials Grosvenor St., Manchester, M1 7HS; Northwestern University School of Medicine, 303 E. Chicago Avenue, Chicago, IL 60611-3008

2016-07-27

The Diamond Beamline I13L is dedicated to imaging on the micron- and nano-lengthscale, operating in the energy range between 6 and 30 keV. For this purpose two independent stations have been built. The imaging branch is fully operational for micro-tomography and in-line phase contrast imaging with micrometer resolution. Currently a full-field microscope providing 50nm spatial resolution over a field of view of 100 µm is being tested. On the coherence branch, coherent diffraction imaging techniques such as ptychography and coherent X-ray Bragg diffraction are currently developed. The beamline contains a number of unique features. The machine layout has been modifiedmore » to the so-called mini-beta scheme, providing significantly increased flux from the two canted undulators. New instrumental designs such as a robot arm for the detector in diffraction experiments have been employed. The imaging branch is operated in collaboration with Manchester University, called therefore the Diamond-Manchester Branchline.« less

Simultaneous nanocalorimetry and fast XRD measurements to study the silicide formation in Pd/a-Si bilayers.

PubMed

Molina-Ruiz, Manel; Ferrando-Villalba, Pablo; Rodríguez-Tinoco, Cristian; Garcia, Gemma; Rodríguez-Viejo, Javier; Peral, Inma; Lopeandía, Aitor F

2015-05-01

The use of a membrane-based chip nanocalorimeter in a powder diffraction beamline is described. Simultaneous wide-angle X-ray scattering and scanning nanocalorimetric measurements are performed on a thin-film stack of palladium/amorphous silicon (Pd/a-Si) at heating rates from 0.1 to 10 K s(-1). The nanocalorimeter works under a power-compensation scheme previously developed by the authors. Kinetic and structural information of the consumed and created phases can be obtained from the combined techniques. The formation of Pd2Si produces a broad calorimetric peak that contains overlapping individual processes. It is shown that Pd consumption precedes the formation of the crystalline Pd2Si phase and that the crystallite size depends on the heating rate of the experiment.

Single-crystal Raman spectroscopy and X-ray crystallography at beamline X26-C of the NSLS

PubMed Central

Stoner-Ma, Deborah; Skinner, John M.; Schneider, Dieter K.; Cowan, Matt; Sweet, Robert M.; Orville, Allen M.

2011-01-01

Three-dimensional structures derived from X-ray diffraction of protein crystals provide a wealth of information. Features and interactions important for the function of macromolecules can be deduced and catalytic mechanisms postulated. Still, many questions can remain, for example regarding metal oxidation states and the interpretation of ‘mystery density’, i.e. ambiguous or unknown features within the electron density maps, especially at ∼2 Å resolutions typical of most macromolecular structures. Beamline X26-C at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory (BNL), provides researchers with the opportunity to not only determine the atomic structure of their samples but also to explore the electronic and vibrational characteristics of the sample before, during and after X-ray diffraction data collection. When samples are maintained under cryo-conditions, an opportunity to promote and follow photochemical reactions in situ as a function of X-ray exposure is also provided. Plans are in place to further expand the capabilities at beamline X26-C and to develop beamlines at NSLS-II, currently under construction at BNL, which will provide users access to a wide array of complementary spectroscopic methods in addition to high-quality X-ray diffraction data. PMID:21169688

New Developments at the ALS High-Pressure Beamline 12.2.2

NASA Astrophysics Data System (ADS)

Kunz, M.; MacDowell, A. A.; Yan, J.; Beavers, C. C. G.; Doran, A.; Williams, Q. C.

2015-12-01

ALS-beamline 12.2.2 celebrated its 10-year anniversary as a beamline collaboratively operated by the ALS and COMPRES. The anniversary coincided with a major rebuild and expansion of its capabilities for in-situ high-pressure and high-temperature X-ray diffraction. A rebuild of the 12.2.2 laser heating table was completed and commissioned in the past year. The new design relies on a vertically positioned small (~1m x 1m) breadboard that is placed perpendicularly to the incident X-ray beam next to the sample stage. Upstream and downstream viewing-, IR-laser and pyrometry-optics are mounted on opposite surfaces of the breadboard. On-line ruby fluorescence optics including a blue diode laser are also mounted on the upstream surface. The much reduced dimensions of the design lead to smaller mechanical lever arms and thus to a significant suppression of vibrations. This was confirmed in the commissioning phase with high-quality optical images (~ 2 μm resolution) as well as a very stable hotspot in DAC samples. A further optimized pyrometry code was cross-calibrated against thermal expansions of Pt and Ta, and was found to agree with those values within experimental uncertainties. Pyrometry relies on imaging the full hot-spot onto a spectrometer and combining the thus obtained average temperature with an intensity map collected at 700 nm to produce a temperature contour map of the entire sample chamber. Besides axial laser heating, double-sided radial laser heating is also being developed and commissioned. The X-ray source of 12.2.2 makes it an ideal station to focus on high-pressure single crystal diffraction. The present set-up operates parasitically with a single rotation axis on the in-situ laser heating powder diffraction sample stage in concert with a fast (15 fps) amorphous silicon/diode array detector. Although this set-up poses limitations with respect to accessible reciprocal space, high pressure single crystal structure solution and refinements of organic compounds incl. anisotropic displacement parameters have been demonstrated. Imminent development plans aim for the installation of a rugged multi-axis diffractometer on its own dedicated end-station in combination with with a compact fast detector on the 2-theta arm. This will be capable of carrying state of the art wide opening angle DAC's (BX90).

A hard X-ray nanoprobe beamline for nanoscale microscopy.

PubMed

Winarski, Robert P; Holt, Martin V; Rose, Volker; Fuesz, Peter; Carbaugh, Dean; Benson, Christa; Shu, Deming; Kline, David; Stephenson, G Brian; McNulty, Ian; Maser, Jörg

2012-11-01

The Hard X-ray Nanoprobe Beamline (or Nanoprobe Beamline) is an X-ray microscopy facility incorporating diffraction, fluorescence and full-field imaging capabilities designed and operated by the Center for Nanoscale Materials and the Advanced Photon Source at Sector 26 of the Advanced Photon Source at Argonne National Laboratory. This facility was constructed to probe the nanoscale structure of biological, environmental and material sciences samples. The beamline provides intense focused X-rays to the Hard X-ray Nanoprobe (or Nanoprobe) which incorporates Fresnel zone plate optics and a precision laser sensing and control system. The beamline operates over X-ray energies from 3 to 30 keV, enabling studies of most elements in the periodic table, with a particular emphasis on imaging transition metals.

A highly modular beamline electrostatic levitation facility, optimized for in situ high-energy x-ray scattering studies of equilibrium and supercooled liquids

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

Mauro, N.A.; Kelton, K.F.

2011-10-27

High-energy x-ray diffraction studies of metallic liquids provide valuable information about structural evolution on the atomic length scale, leading to insights into the origin of the nucleation barrier and the processes of supercooling and glass formation. The containerless processing of the beamline electrostatic levitation (BESL) facility allows coordinated thermophysical and structural studies of equilibrium and supercooled liquids to be made in a contamination-free, high-vacuum ({approx}10{sup -8} Torr) environment. To date, the incorporation of electrostatic levitation facilities into synchrotron beamlines has been difficult due to the large footprint of the apparatus and the difficulties associated with its transportation and implementation. Here,more » we describe a modular levitation facility that is optimized for diffraction studies of high-temperature liquids at high-energy synchrotron beamlines. The modular approach used in the apparatus design allows it to be easily transported and quickly setup. Unlike most previous electrostatic levitation facilities, BESL can be operated by a single user instead of a user team.« less

Characterising the large coherence length at diamond’s beamline I13L

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

Wagner, U. H., E-mail: ulrich.wagner@diamond.ac.uk; Parsons, A.; Rahomaki, J.

2016-07-27

I13 is a 250 m long hard x-ray beamline (6 keV to 35 keV) at the Diamond Light Source. The beamline comprises of two independent experimental endstations: one for imaging in direct space using x-ray microscopy and one for imaging in reciprocal space using coherent diffraction based imaging techniques [1]. An outstanding feature of the coherence branch, due to its length and a new generation of ultra-stable beamline instrumentation [2], is its capability of delivering a very large coherence length well beyond 200 μm, providing opportunities for unique x-ray optical experiments. In this paper we discuss the challenges of measuringmore » a large coherence length and present quantitative measurement based on analyzing diffraction patterns from a boron fiber [3]. We also discuss the limitations of this classical method in respect to detector performance, very short and long coherence lengths. Furthermore we demonstrate how a Ronchi grating setup [4] can be used to quickly establish if the beam is coherent over a large area.« less

Coherence Length and Vibrations of the Coherence Beamline I13 at the Diamond Light Source

NASA Astrophysics Data System (ADS)

Wagner, U. H.; Parson, A.; Rau, C.

2017-06-01

I13 is a 250 m long hard x-ray beamline for imaging and coherent diffraction at the Diamond Light Source. The beamline (6 keV to 35 keV) comprises two independent experimental endstations: one for imaging in direct space using x-ray microscopy and one for imaging in reciprocal space using coherent diffraction based imaging techniques [1]. In particular the coherence experiments pose very high demands on the performance on the beamline instrumentation, requiring extensive testing and optimisation of each component, even during the assembly phase. Various aspects like the quality of optical components, the mechanical design concept, vibrations, drifts, thermal influences and the performance of motion systems are of particular importance. In this paper we study the impact of the front-end slit size (FE slit size), which determines the horizontal source size, onto the coherence length and the detrimental impact of monochromator vibrations using in-situ x-ray metrology in conjunction with fringe visibility measurements and vibration measurements, based on centroid tracking of an x-ray pencil beam with a photon-counting detector.

In-situ Diffraction Study of Magnetite at Simultaneous High Pressure and High Temperature Using Synchrotron Radiation

NASA Astrophysics Data System (ADS)

Wang, L.; Zhang, J.; Wang, S.; Chen, H.; Zhao, Y.

2014-12-01

Magnetite intertwined with the evolution of human civilizations, and remains so today. It is technologically and scientifically important by virtue of its unique magnetic and electrical properties. Magnetite is a common mineral found in a variety of geologic environments, and plays an important role in deciphering the oxygen evolution in the Earth's atmosphere and its deep interiors. The latter application asks for the knowledge of the thermal and elastic properties of magnetite at high pressures and temperatures, which is currently not available in literature. We have carried out a few in-situ diffraction experiments on magnetite using white synchrotron radiation at beamline X17B2 of National Synchrotron Light Source (NSLS). A DIA module in an 1100-ton press and WC anvils were employed for compression, and diffraction spectra were collected at simultaneous high pressures (P) and temperatures (T) (up to 9 GPa and 900 oC). Mixture of amorphous boron and epoxy resin was used as pressure medium, and NaCl as pressure marker. Temperature was recorded by W-Re thermocouples. Commercially purchased magnetite powder and a mixture of the said powder and NaCl (1:1) were used as starting material in separate experiments. Preliminary data analyses have yielded following observations: (1) Charge disordering seen at ambient pressure remains active in current experiments, especially at lower pressures (< 6 GPa); (2) Though at each condition potentially complicated by charge disordering process, isothermal compression curves remains simple and reproducible; (3) During cooling, the reversibility and degree of cation disordering depend on the starting material and/or experimental P-T path; and (4) cation disordering notably reduces the apparent bulk moduli of magnetite.

MX2: a high-flux undulator microfocus beamline serving both the chemical and macromolecular crystallography communities at the Australian Synchrotron

PubMed Central

Aishima, Jun; Cherukuvada, Hima; Clarken, Robert; Clift, Mark; Ericsson, Daniel Jesper; Macedo, Sofia; Mudie, Nathan; Price, Jason Roy; Rostan, Robert; Williamson, Rachel

2018-01-01

MX2 is an in-vacuum undulator-based crystallography beamline at the 3 GeV Australian Synchrotron. The beamline delivers hard X-rays in the energy range 4.8–21 keV to a focal spot of 22 × 12 µm FWHM (H × V). At 13 keV the flux at the sample is 3.4 × 1012 photons s−1. The beamline endstation allows robotic handling of cryogenic samples via an updated SSRL SAM robot. This beamline is ideal for weakly diffracting hard-to-crystallize proteins, virus particles, protein assemblies and nucleic acids as well as smaller molecules such as inorganic catalysts and organic drug molecules. The beamline is now mature and has enjoyed a full user program for the last nine years. This paper describes the beamline status, plans for its future and some recent scientific highlights. PMID:29714201

MxCuBE: a synchrotron beamline control environment customized for macromolecular crystallography experiments

PubMed Central

Gabadinho, José; Beteva, Antonia; Guijarro, Matias; Rey-Bakaikoa, Vicente; Spruce, Darren; Bowler, Matthew W.; Brockhauser, Sandor; Flot, David; Gordon, Elspeth J.; Hall, David R.; Lavault, Bernard; McCarthy, Andrew A.; McCarthy, Joanne; Mitchell, Edward; Monaco, Stéphanie; Mueller-Dieckmann, Christoph; Nurizzo, Didier; Ravelli, Raimond B. G.; Thibault, Xavier; Walsh, Martin A.; Leonard, Gordon A.; McSweeney, Sean M.

2010-01-01

The design and features of a beamline control software system for macromolecular crystallography (MX) experiments developed at the European Synchrotron Radiation Facility (ESRF) are described. This system, MxCuBE, allows users to easily and simply interact with beamline hardware components and provides automated routines for common tasks in the operation of a synchrotron beamline dedicated to experiments in MX. Additional functionality is provided through intuitive interfaces that enable the assessment of the diffraction characteristics of samples, experiment planning, automatic data collection and the on-line collection and analysis of X-ray emission spectra. The software can be run in a tandem client-server mode that allows for remote control and relevant experimental parameters and results are automatically logged in a relational database, ISPyB. MxCuBE is modular, flexible and extensible and is currently deployed on eight macromolecular crystallography beamlines at the ESRF. Additionally, the software is installed at MAX-lab beamline I911-3 and at BESSY beamline BL14.1. PMID:20724792

A hard X-ray nanoprobe beamline for nanoscale microscopy

PubMed Central

Winarski, Robert P.; Holt, Martin V.; Rose, Volker; Fuesz, Peter; Carbaugh, Dean; Benson, Christa; Shu, Deming; Kline, David; Stephenson, G. Brian; McNulty, Ian; Maser, Jörg

2012-01-01

The Hard X-ray Nanoprobe Beamline (or Nanoprobe Beamline) is an X-ray microscopy facility incorporating diffraction, fluorescence and full-field imaging capabilities designed and operated by the Center for Nanoscale Materials and the Advanced Photon Source at Sector 26 of the Advanced Photon Source at Argonne National Laboratory. This facility was constructed to probe the nanoscale structure of biological, environmental and material sciences samples. The beamline provides intense focused X-rays to the Hard X-ray Nanoprobe (or Nanoprobe) which incorporates Fresnel zone plate optics and a precision laser sensing and control system. The beamline operates over X-ray energies from 3 to 30 keV, enabling studies of most elements in the periodic table, with a particular emphasis on imaging transition metals. PMID:23093770

Nanoscopium: a Scanning Hard X-ray Nanoprobe Beamline at Synchrotron Soleil

NASA Astrophysics Data System (ADS)

Somogyi, A.; Polack, F.; Moreno, T.

2010-06-01

Nanoscopium is the single scanning hard X-ray nano-probe beamline planned at SOLEIL. This ˜155 m long beamline will fully exploit the high brilliance and coherence characteristics of the X-ray beam both for diffraction limited focusing and for contrast formation. It will offer the most advanced imaging techniques in multimodal mode and will be a research tool for a wide user community working in the fields of earth-, environmental-, and life-sciences. The different μ-μnano-probe techniques offered by the beamline will permit elemental mapping at trace (ppm) levels (scanning XRF), speciation mapping (XANES), phase gradient mapping (scanning differential phase contrast), and density-contrast based imaging of internal structures (coherent diffraction imaging) in the 30 nm to 1 μm spatial resolution range, also in "in situ conditions". Nanoscopium will cover the 5-20 keV energy range. The stability of the nanobeam will be ensured by horizontally reflecting beamline optics (a sagitally and a tangentially pre-focusing mirror, horizontally reflecting monochromators) in front of the overfilled secondary source. Trade-off between high energy resolution (ΔE/E˜10-4) and high flux (1011 ph/s with ΔE/E˜10-2) will be achieved by two interchangeable monochromators (a double crystal and a double multilayer one). KB mirror and FZP lenses will be used as focusing devices. The beamline is in the design and construction phase. It is foreseen to be open for users at the beginning of 2013.

X-ray optical simulations supporting advanced commissioning of the coherent hard x-ray beamline at NSLS-II

NASA Astrophysics Data System (ADS)

Wiegart, L.; Rakitin, M.; Fluerasu, A.; Chubar, O.

2017-08-01

We present the application of fully- and partially-coherent synchrotron radiation wavefront propagation simulation functions, implemented in the "Synchrotron Radiation Workshop" computer code, to create a `virtual beamline' mimicking the Coherent Hard X-ray scattering beamline at NSLS-II. The beamline simulation includes all optical beamline components, such as the insertion device, mirror with metrology data, slits, double crystal monochromator and refractive focusing elements (compound refractive lenses and kinoform lenses). A feature of this beamline is the exploitation of X-ray beam coherence, boosted by the low-emittance NSLS-II storage-ring, for techniques such as X-ray Photon Correlation Spectroscopy or Coherent Diffraction Imaging. The key performance parameters are the degree of Xray beam coherence and photon flux, and the trade-off between them needs to guide the beamline settings for specific experimental requirements. Simulations of key performance parameters are compared to measurements obtained during beamline commissioning, and include the spectral flux of the undulator source, the degree of transverse coherence as well as focal spot sizes.

Aladdin: Transforming science at SRC

NASA Astrophysics Data System (ADS)

Bisognano, J.; Bissen, M.; Green, M.; Jacobs, K.; Moore, C.; Olson, E.; Severson, M.; Wehlitz, R.

2011-09-01

The Synchrotron Radiation Center (SRC) is dedicated to enabling of innovative research using IR, ultraviolet, and soft X-ray synchrotron radiation. It delivers beam time with high reliability (99%) and continues to improve the Aladdin storage ring complex. A lower emittance tuning has been commissioned to support a microfocus capability. SRC successfully installed an APPLE II undulator providing elliptically polarized light with lattice compensation for flexible scanning. Installation of a new IR beamline at SRC is providing synchrotron chemical imaging with unprecedented structural and chemical information, simultaneously. In addition, SRC has established a strong education and outreach program to bring the knowledge and power of light source science to a wider national community. It is moving forward into the future by developing a new micro focus beamline producing a diffraction-limited focus of about 500 nm at 22 eV, proposing an additional diffraction-limited chemical imaging beamline, and advancing the Wisconsin Free Electron Laser (WiFEL) concept.

A next-generation in-situ nanoprobe beamline for the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Maser, Jörg; Lai, Barry; Buonassisi, Tonio; Cai, Zhonghou; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Harder, Ross; Jacobsen, Chris; Liu, Wenjun; Murray, Conal; Preissner, Curt; Roehrig, Chris; Rose, Volker; Shu, Deming; Vine, David; Vogt, Stefan

2013-09-01

The Advanced Photon Source is currently developing a suite of new hard x-ray beamlines, aimed primarily at the study of materials and devices under real conditions. One of the flagship beamlines of the APS Upgrade is the In-Situ Nanoprobe beamline (ISN beamline), which will provide in-situ and operando characterization of advanced energy materials and devices under change of temperature and gases, under applied fields, in 3D. The ISN beamline is designed to deliver spatially coherent x-rays with photon energies between 4 keV and 30 keV to the ISN instrument. As an x-ray source, a revolver-type undulator with two interchangeable magnetic structures, optimized to provide high brilliance throughout the range of photon energies of 4 keV - 30 keV, will be used. The ISN instrument will provide a smallest hard x-ray spot of 20 nm using diffractive optics, with sensitivity to sub-10 nm sample structures using coherent diffraction. Using nanofocusing mirrors in Kirkpatrick-Baez geometry, the ISN will also provide a focus of 50 nm with a flux of 8·1011 Photons/s at a photon energy of 10 keV, several orders of magnitude larger than what is currently available. This will allow imaging of trace amounts of most elements in the periodic table, with a sensitivity to well below 100 atoms for most metals in thin samples. It will also enable nanospectroscopic studies of the chemical state of most materials relevant to energy science. The ISN beamline will be primarily used to study inorganic and organic photovoltaic systems, advanced batteries and fuel cells, nanoelectronics devices, and materials and systems diesigned to reduce the environmental impact of combustion.

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

Amemiya, Kenta; Toyoshima, Akio; Kikuchi, Takashi

The design and commissioning of a new soft X-ray beamline, BL-16A, at the Photon Factory is presented. The beamline consists of a pre-focusing mirror, an entrance slit, a variable-included-angle varied-line-spacing plane grating monochromator, and a post-focusing system as usual, and provides circularly and linearly polarized soft X rays in the energy range 200-1500 eV with an APPLE-II type undulator. The commissioning procedure for the beamline optics is described in detail, especially the check of the focal position for the zero-th order and diffracted X rays.

Quantitative evaluation of bone-mineral density loss using X-ray coherent scattering

NASA Astrophysics Data System (ADS)

Barroso, Regina Cély; Oliveira, Luis Fernando; Castro, Carlos Roberto Ferreira; Lima, João Carlos; Braz, Delson; Lopes, Ricardo Tadeu; Droppa, Roosevel; Tromba, Giuliana; Mancini, Lucia; Zanini, Franco; Rigon, Luigi; Dreossi, Diego

2007-08-01

In this work, we intend to relate the mineral to non-mineral bone scattering intensity ratio with the bone-mineral density (BMD) reduction. In this way, EDXRD can be a novel technique to measure BMD loss in function of the mineral and non-mineral scattering intensity. The scattering profiles were obtained at Laboratório Nacional de Luz Síncrotron (LNLS) at the X-ray diffraction beamline XD2. A double-crystal Si(1 1 1) pre-monochromator, upstream of the beamline, was used to select a small energy bandwidth (Δ λ/ λ≈10 -4) at 11 keV. The sample holder has a circle depression in the center to contain a range of bone and fat mixture ratios. The mixture consists of powdered cortical bone and fat, which together simulate in vivo bone. The diffraction patterns were carried out with 0.5 mm slits after and behind of the sample holder. The data were collected in 0.05° increments every 0.5 s. EDXRD results show an indication of different bone densities may be distinguished which suggested that X-ray coherent scattering technique may have a role in monitoring changes in BMD via changes in the related scattering intensity of mineral and non-mineral bone. The main aim of the Synchrotron Radiation for MEdical Physics (SYRMEP) project at the ELETTRA is the investigation and the development of innovative techniques for medical imaging. The beamline provides, at a distance of about 23 m from the source, a monochromatic, laminar section X-ray beam with a maximum area of about 160×5 mm 2 at 20 keV. The monochromator, that covers the entire angular acceptance of the beamline, is based on a double-Si (1 1 1) crystal system working in Bragg configuration. A micrometric vertical and horizontal translation stage allows the positioning and scanning of the sample with respect to the stationary beam. In this case, the detector is kept stationary in front of the beam, while the object is rotated in discrete steps in front of it. At each rotation, a projection is acquired. A goniometric double-cradle system is used to adjust the rotation axis, which must be orthogonal with respect to the detector plane in transmission computed tomography (CT). The samples consisted of a 8 mm cube of bovine bone surrounded of a cartilage interface. High-resolution images of the trabecular structure were obtained by means a 16-bit CCD camera, 2048×2048 pixels, 14 μm pixel size (maximum spatial resolution: 25 μm).

The Structural Biology Center 19ID undulator beamline: facility specifications and protein crystallographic results

PubMed Central

Rosenbaum, Gerd; Alkire, Randy W.; Evans, Gwyndaf; Rotella, Frank J.; Lazarski, Krzystof; Zhang, Rong-Guang; Ginell, Stephan L.; Duke, Norma; Naday, Istvan; Lazarz, Jack; Molitsky, Michael J.; Keefe, Lisa; Gonczy, John; Rock, Larry; Sanishvili, Ruslan; Walsh, Martin A.; Westbrook, Edwin; Joachimiak, Andrzej

2008-01-01

The 19ID undulator beamline of the Structure Biology Center has been designed and built to take full advantage of the high flux, brilliance and quality of X-ray beams delivered by the Advanced Photon Source. The beamline optics are capable of delivering monochromatic X-rays with photon energies from 3.5 to 20 keV (3.5–0.6 Å wavelength) with fluxes up to 8–18 × 1012 photons s−1 (depending on photon energy) onto cryogenically cooled crystal samples. The size of the beam (full width at half-maximum) at the sample position can be varied from 2.2 mm × 1.0 mm (horizontal × vertical, unfocused) to 0.083 mm × 0.020 mm in its fully focused configuration. Specimen-to-detector distances of between 100 mm and 1500 mm can be used. The high flexibility, inherent in the design of the optics, coupled with a κ-geometry goniometer and beamline control software allows optimal strategies to be adopted in protein crystallographic experiments, thus maximizing the chances of their success. A large-area mosaic 3 × 3 CCD detector allows high-quality diffraction data to be measured rapidly to the crystal diffraction limits. The beamline layout and the X-ray optical and endstation components are described in detail, and the results of representative crystallographic experiments are presented. PMID:16371706

Characterization of Beryllium Windows Using Coherent X-rays at 1-km Beamline

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

Goto, Shunji; Yabashi, Makina; Takahashi, Sunao

2004-05-12

Beryllium windows were characterized using coherent x-rays at the one-kilometer beamline of SPring-8. Non-uniformity of transmission x-ray images is largely due to Fresnel diffraction from deficiencies such as surface pits with diameter of order of one micron to ten microns, having no correlation with averaged surface roughness measured with an optical profilometer.

Development and calibration of mirrors and gratings for the Soft X-ray materials science beamline at the Linac Coherent Light Source free-electron laser

DOE PAGES

Soufli, Regina; Fernandez-Perea, Monica; Baker, Sherry L.; ...

2012-04-18

This article discusses the development and calibration of the x-ray reflective and diffractive elements for the Soft X-ray Materials Science (SXR) beamline of the Linac Coherent Light Source (LCLS) free-electron laser (FEL), designed for operation in the 500 – 2000 eV region. The surface topography of three Si mirror substrates and two Si diffraction grating substrates was examined by atomic force microscopy (AFM) and optical profilometry. The figure of the mirror substrates was also verified via surface slope measurements with a long trace profiler. A boron carbide (B 4C) coating especially optimized for the LCLS FEL conditions was deposited onmore » all SXR mirrors and gratings. Coating thickness uniformity of 0.14 nm root mean square (rms) across clear apertures extending to 205 mm length was demonstrated for all elements, as required to preserve the coherent wavefront of the LCLS source. The reflective performance of the mirrors and the diffraction efficiency of the gratings were calibrated at beamline 6.3.2 at the Advanced Light Source synchrotron. To verify the integrity of the nanometer-scale grating structure, the grating topography was examined by AFM before and after coating. This is to our knowledge the first time B 4C-coated diffraction gratings are demonstrated for operation in the soft x-ray region.« less

Focusing, collimation and flux throughput at the IMCA-CAT bending-magnet beamline at the Advanced Photon Source

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

Koshelev, Irina; Huang, Rong; Graber, Timothy

2009-09-02

The IMCA-CAT bending-magnet beamline was upgraded with a collimating mirror in order to achieve the energy resolution required to conduct high-quality multi- and single-wavelength anomalous diffraction (MAD/SAD) experiments without sacrificing beamline flux throughput. Following the upgrade, the bending-magnet beamline achieves a flux of 8 x 10{sup 11} photons s{sup -1} at 1 {angstrom} wavelength, at a beamline aperture of 1.5 mrad (horizontal) x 86 {mu}rad (vertical), with energy resolution (limited mostly by the intrinsic resolution of the monochromator optics) {delta}E/E = 1.5 x 10{sup -4} (at 10 kV). The beamline operates in a dynamic range of 7.5-17.5 keV and deliversmore » to the sample focused beam of size (FWHM) 240 {micro}m (horizontally) x 160 {micro}m (vertically). The performance of the 17-BM beamline optics and its deviation from ideally shaped optics is evaluated in the context of the requirements imposed by the needs of protein crystallography experiments. An assessment of flux losses is given in relation to the (geometric) properties of major beamline components.« less

Geometrical layout and optics modelling of the surface science beamline station at the SESAME synchrotron radiation facility.

PubMed

Salah, Wa'el; Sanchez del Rio, Manuel

2011-05-01

The layout and the optical performance of the SGM branch of the D09 bending-magnet beamline, under construction at SESAME, are presented. The beamline is based on the Dragon-type design and delivers photons over the spectral range 15-250 eV. One fixed entrance slit and a movable exit slit are used. The performance of the beamline has been characterized by calculating the mirror reflectivities and the grating efficiencies. The flux and resolution were calculated by ray-tracing using SHADOW. The grating diffraction efficiencies were calculated using the GRADIF code. The results and the overall shapes of the predicted curves are in reasonable agreement with those obtained using an analytical formula.

High Pressure Single Crystal Diffraction at PX 2

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

Zhang, Dongzhou; Dera, Przemyslaw K.; Eng, Peter J.

2017-01-01

In this report, we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell at the GSECARS 13-BM-C beamline at the Advanced Photon Source. ATREX and RSV programs are used to analyze the data.

Facilities for small-molecule crystallography at synchrotron sources.

PubMed

Barnett, Sarah A; Nowell, Harriott; Warren, Mark R; Wilcox, Andrian; Allan, David R

2016-01-01

Although macromolecular crystallography is a widely supported technique at synchrotron radiation facilities throughout the world, there are, in comparison, only very few beamlines dedicated to small-molecule crystallography. This limited provision is despite the increasing demand for beamtime from the chemical crystallography community and the ever greater overlap between systems that can be classed as either small macromolecules or large small molecules. In this article, a very brief overview of beamlines that support small-molecule single-crystal diffraction techniques will be given along with a more detailed description of beamline I19, a dedicated facility for small-molecule crystallography at Diamond Light Source.

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

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

Murray, Thomas D.; Johns Hopkins University School of Medicine, Baltimore, MD 21205; Lyubimov, Artem Y.

A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. 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 themore » 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 (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. 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

Recent Major Improvements to the ALS Sector 5 MacromolecularCrystallography Beamlines

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

Morton, Simon A.; Glossinger, James; Smith-Baumann, Alexis

2007-07-01

Although the Advanced Light Source (ALS) was initially conceived primarily as a low energy (1.9GeV) 3rd generation source of VUV and soft x-ray radiation it was realized very early in the development of the facility that a multipole wiggler source coupled with high quality, (brightness preserving), optics would result in a beamline whose performance across the optimal energy range (5-15keV) for macromolecular crystallography (MX) would be comparable to, or even exceed, that of many existing crystallography beamlines at higher energy facilities. Hence, starting in 1996, a suite of three beamlines, branching off a single wiggler source, was constructed, which togethermore » formed the ALS Macromolecular Crystallography Facility. From the outset this facility was designed to cater equally to the needs of both academic and industrial users with a heavy emphasis placed on the development and introduction of high throughput crystallographic tools, techniques, and facilities--such as large area CCD detectors, robotic sample handling and automounting facilities, a service crystallography program, and a tightly integrated, centralized, and highly automated beamline control environment for users. This facility was immediately successful, with the primary Multiwavelength Anomalous Diffraction beamline (5.0.2) in particular rapidly becoming one of the foremost crystallographic facilities in the US--responsible for structures such as the 70S ribosome. This success in-turn triggered enormous growth of the ALS macromolecular crystallography community and spurred the development of five additional ALS MX beamlines all utilizing the newly developed superconducting bending magnets ('superbends') as sources. However in the years since the original Sector 5.0 beamlines were built the performance demands of macromolecular crystallography users have become ever more exacting; with growing emphasis placed on studying larger complexes, more difficult structures, weakly diffracting or smaller crystals, and on more rapidly screening larger numbers of candidate crystals; all of these requirements translate directly into a pressing need for increased flux, a tighter beam focus and faster detectors. With these growing demands in mind a major program of beamline and detector upgrades was initiated in 2004 with the goal of dramatically enhancing all aspects of beamline performance. Approximately $3 million in funding from diverse sources including NIH, LBL, the ALS, and the industrial and academic members of the beamline Participating Research Team (PRT), has been employed to develop and install new high performance beamline optics and to purchase the latest generation of CCD detectors. This project, which reached fruition in early 2007, has now fulfilled all of its original goals--boosting the flux on all three beamlines by up to 20-fold--with a commensurate reduction in exposure and data acquisition times for users. The performance of the Sector 5.0 beamlines is now comparable to that of the latest generation ALS superbend beamlines and, in the case of beamline 5.0.2, even surpasses it by a considerable margin. Indeed, the present performance of this beamline is now, once again, comparable to that envisioned for many MX beamlines planned or under construction on newer or higher energy machines.« less

Coherent Soft X-ray Diffraction Imaging of Coliphage PR772 at the Linac Coherent Light Source

DOE Data Explorer

Reddy, Hemanth, K.N.

2017-01-05

A dataset of coherent soft X-ray diffraction images of Coliphage PR772 virus, collected at the Atomic Molecular Optics (AMO) beamline with pnCCD detectors in the LAMP instrument at the Linac Coherent Light Source.

A Next-Generation Hard X-Ray Nanoprobe Beamline for In Situ Studies of Energy Materials and Devices

NASA Astrophysics Data System (ADS)

Maser, Jörg; Lai, Barry; Buonassisi, Tonio; Cai, Zhonghou; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Jacobsen, Chris; Preissner, Curt; Roehrig, Chris; Rose, Volker; Shu, Deming; Vine, David; Vogt, Stefan

2014-01-01

The Advanced Photon Source is developing a suite of new X-ray beamlines to study materials and devices across many length scales and under real conditions. One of the flagship beamlines of the APS upgrade is the In Situ Nanoprobe (ISN) beamline, which will provide in situ and operando characterization of advanced energy materials and devices under varying temperatures, gas ambients, and applied fields, at previously unavailable spatial resolution and throughput. Examples of materials systems include inorganic and organic photovoltaic systems, advanced battery systems, fuel cell components, nanoelectronic devices, advanced building materials and other scientifically and technologically relevant systems. To characterize these systems at very high spatial resolution and trace sensitivity, the ISN will use both nanofocusing mirrors and diffractive optics to achieve spots sizes as small as 20 nm. Nanofocusing mirrors in Kirkpatrick-Baez geometry will provide several orders of magnitude increase in photon flux at a spatial resolution of 50 nm. Diffractive optics such as zone plates and/or multilayer Laue lenses will provide a highest spatial resolution of 20 nm. Coherent diffraction methods will be used to study even small specimen features with sub-10 nm relevant length scale. A high-throughput data acquisition system will be employed to significantly increase operations efficiency and usability of the instrument. The ISN will provide full spectroscopy capabilities to study the chemical state of most materials in the periodic table, and enable X-ray fluorescence tomography. In situ electrical characterization will enable operando studies of energy and electronic devices such as photovoltaic systems and batteries. We describe the optical concept for the ISN beamline, the technical design, and the approach for enabling a broad variety of in situ studies. We furthermore discuss the application of hard X-ray microscopy to study defects in multi-crystalline solar cells, one of the lines of inquiries for which the ISN is being developed.

Sequential x-ray diffraction topography at 1-BM x-ray optics testing beamline at the advanced photon source

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

Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Shvyd’ko, Yuri; Trakhtenberg, Emil

2016-07-27

We report progress on implementation and commissioning of sequential X-ray diffraction topography at 1-BM Optics Testing Beamline of the Advanced Photon Source to accommodate growing needs of strain characterization in diffractive crystal optics and other semiconductor single crystals. The setup enables evaluation of strain in single crystals in the nearly-nondispersive double-crystal geometry. Si asymmetric collimator crystals of different crystallographic orientations were designed, fabricated and characterized using in-house capabilities. Imaging the exit beam using digital area detectors permits rapid sequential acquisition of X-ray topographs at different angular positions on the rocking curve of a crystal under investigation. Results on sensitivity andmore » spatial resolution are reported based on experiments with high-quality Si and diamond crystals. The new setup complements laboratory-based X-ray topography capabilities of the Optics group at the Advanced Photon Source.« less

The use of workflows in the design and implementation of complex experiments in macromolecular crystallography.

PubMed

Brockhauser, Sandor; Svensson, Olof; Bowler, Matthew W; Nanao, Max; Gordon, Elspeth; Leal, Ricardo M F; Popov, Alexander; Gerring, Matthew; McCarthy, Andrew A; Gotz, Andy

2012-08-01

The automation of beam delivery, sample handling and data analysis, together with increasing photon flux, diminishing focal spot size and the appearance of fast-readout detectors on synchrotron beamlines, have changed the way that many macromolecular crystallography experiments are planned and executed. Screening for the best diffracting crystal, or even the best diffracting part of a selected crystal, has been enabled by the development of microfocus beams, precise goniometers and fast-readout detectors that all require rapid feedback from the initial processing of images in order to be effective. All of these advances require the coupling of data feedback to the experimental control system and depend on immediate online data-analysis results during the experiment. To facilitate this, a Data Analysis WorkBench (DAWB) for the flexible creation of complex automated protocols has been developed. Here, example workflows designed and implemented using DAWB are presented for enhanced multi-step crystal characterizations, experiments involving crystal reorientation with kappa goniometers, crystal-burning experiments for empirically determining the radiation sensitivity of a crystal system and the application of mesh scans to find the best location of a crystal to obtain the highest diffraction quality. Beamline users interact with the prepared workflows through a specific brick within the beamline-control GUI MXCuBE.

Exploring Jupiter's icy moons with old techniques and big facilities - new insights on sulfuric acid hydrates

NASA Astrophysics Data System (ADS)

Maynard-Casely, H. E.; Avdeev, M.; Brand, H.; Wallwork, K.

2013-12-01

Sulfuric acid hydrates have been proposed to be abundant on the surface of Europa [1], and hence would be important planetary forming materials for this moon and its companions Ganymede and Callisto. Understanding of the surface features and subsurface of these moons could be advanced by firmer knowledge of the icy materials that comprise them [2], insight into which can be drawn from firmer knowledge of physical properties and phase behaviour of the candidate materials. We wish to present results from a study that started with the question ';What form of sulfuric acid hydrate would form on the surface of Europa'. The intrinsic hydrogen-domination of planetary ices, makes studying these materials with laboratory powder diffraction very challenging. Insights into their crystalline phase behavior and the extraction of a number of thermal and mechanical properties is often only accessible with high-flux synchrotron x-ray diffraction and utilization of the large scattering cross section with neutron diffraction. We have used the Powder Diffraction beamline at Australian synchrotron [4] and the Echidna (High-resolution neutron powder diffraction) instrument of the Australian Nuclear Science and Technology Organization, [5] to obtain an number of new insights into the crystalline phases formed from sulfruic acid and water mixtures. These instruments have enabled the discovery a new water-rich sulfuric acid hydrate form [6], improved structural characterisation of existing forms [7] and a charting the phase diagram of this fundamental binary system [8]. This has revealed exciting potential for understanding more about the surface of Europa from space, perhaps even providing a window into its past. [1] Carlson, R.W., R.E. Johnson, and M.S. Anderson, Science, 1999. 286(5437): p. 97-99. [2] Fortes, A.D. and M. Choukroun. Space Sci Rev, 2010. 153(1-4): p. 185-218. [3] Blake, D., et al., Space Sci Rev,, 2012. 170(1-4): p. 341-399. [4] Wallwork, K.S., Kennedy B. J. and Wang, D., AIP Conf Proc, 2007. 879: p. 879-882. [5] Liss, K.D., et al., Phys B-Cond Mat, 2006. 385-86: p. 1010-1012. [6] Maynard-Casely, H.E., K.S. Wallwork, and M. Avdeev, (In review). [7] Maynard-Casely, H.E., H.E.A. Brand, and K.S. Wallwork, J.of App.Cryst, 2012. 45: p.1198-1207. [8] Maynard-Casely, H.E., K.S. Wallwork, and H.E.A. Brand, (In Preparation). Stages of the crystal structure determination of sulfruic acid octahydrate a) the oxygen and sulfur postions were determined from the synchrotron x-ray data b) Once neutron diffraction data was collected Fourier difference methods were used to locate hydrogen positions to determine c) the full structure of sulfuric acid octahydrate.

Development of a synchrotron biaxial tensile device for in situ characterization of thin films mechanical response.

PubMed

Geandier, G; Thiaudière, D; Randriamazaoro, R N; Chiron, R; Djaziri, S; Lamongie, B; Diot, Y; Le Bourhis, E; Renault, P O; Goudeau, P; Bouaffad, A; Castelnau, O; Faurie, D; Hild, F

2010-10-01

We have developed on the DIFFABS-SOLEIL beamline a biaxial tensile machine working in the synchrotron environment for in situ diffraction characterization of thin polycrystalline films mechanical response. The machine has been designed to test compliant substrates coated by the studied films under controlled, applied strain field. Technological challenges comprise the sample design including fixation of the substrate ends, the related generation of a uniform strain field in the studied (central) volume, and the operations from the beamline pilot. Preliminary tests on 150 nm thick W films deposited onto polyimide cruciform substrates are presented. The obtained results for applied strains using x-ray diffraction and digital image correlation methods clearly show the full potentialities of this new setup.

High throughput screening of ligand binding to macromolecules using high resolution powder diffraction

DOEpatents

Von Dreele, Robert B.; D'Amico, Kevin

2006-10-31

A process is provided for the high throughput screening of binding of ligands to macromolecules using high resolution powder diffraction data including producing a first sample slurry of a selected polycrystalline macromolecule material and a solvent, producing a second sample slurry of a selected polycrystalline macromolecule material, one or more ligands and the solvent, obtaining a high resolution powder diffraction pattern on each of said first sample slurry and the second sample slurry, and, comparing the high resolution powder diffraction pattern of the first sample slurry and the high resolution powder diffraction pattern of the second sample slurry whereby a difference in the high resolution powder diffraction patterns of the first sample slurry and the second sample slurry provides a positive indication for the formation of a complex between the selected polycrystalline macromolecule material and at least one of the one or more ligands.

The use of a mini-κ goniometer head in macromolecular crystallography diffraction experiments

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

Brockhauser, Sandor; UJF–EMBL–CNRS UMI 3265, 6 Rue Jules Horowitz, 38043 Grenoble; Ravelli, Raimond B. G.

2013-07-01

Hardware and software solutions for MX data-collection strategies using the EMBL/ESRF miniaturized multi-axis goniometer head are presented. Most macromolecular crystallography (MX) diffraction experiments at synchrotrons use a single-axis goniometer. This markedly contrasts with small-molecule crystallography, in which the majority of the diffraction data are collected using multi-axis goniometers. A novel miniaturized κ-goniometer head, the MK3, has been developed to allow macromolecular crystals to be aligned. It is available on the majority of the structural biology beamlines at the ESRF, as well as elsewhere. In addition, the Strategy for the Alignment of Crystals (STAC) software package has been developed to facilitatemore » the use of the MK3 and other similar devices. Use of the MK3 and STAC is streamlined by their incorporation into online analysis tools such as EDNA. The current use of STAC and MK3 on the MX beamlines at the ESRF is discussed. It is shown that the alignment of macromolecular crystals can result in improved diffraction data quality compared with data obtained from randomly aligned crystals.« less

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

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

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

Development of a synchrotron biaxial tensile device for in situ characterization of thin films mechanical response

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

Geandier, G.; Synchrotron SOLEIL, L'Orme des Merisiers, BP 48, 91192 Gif sur Yvette; LPMTM, UPR 9001 CNRS, Universite Paris-Nord, 93430 Villetaneuse

2010-10-15

We have developed on the DIFFABS-SOLEIL beamline a biaxial tensile machine working in the synchrotron environment for in situ diffraction characterization of thin polycrystalline films mechanical response. The machine has been designed to test compliant substrates coated by the studied films under controlled, applied strain field. Technological challenges comprise the sample design including fixation of the substrate ends, the related generation of a uniform strain field in the studied (central) volume, and the operations from the beamline pilot. Preliminary tests on 150 nm thick W films deposited onto polyimide cruciform substrates are presented. The obtained results for applied strains usingmore » x-ray diffraction and digital image correlation methods clearly show the full potentialities of this new setup.« less

High-throughput and in situ EDXRD investigation on the formation of two new metal aminoethylphosphonates - Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) and Ca(OH)(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3}){center_dot}2H{sub 2}O

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

Schmidt, Corinna; Feyand, Mark; Rothkirch, Andre

2012-04-15

The system Ca{sup 2+}/2-aminoethylphosphonic acid/H{sub 2}O/NaOH was systematically investigated using high-throughput methods. The experiments led to one new compound Ca(O{sub 3}PC{sub 2} H{sub 4}NH{sub 2}) (1) and the crystal structure was determined using in house X-ray powder diffraction data (monoclinic, P2{sub 1}/c, a=9.7753(3), b=6.4931(2), c=8.4473(2) A, {beta}=106.46(2) Degree-Sign , V=514.20(2) A{sup 3}, Z=4). The formation of 1 was investigated by in situ energy dispersive X-ray diffraction measurements (EDXRD) at beamline F3 at HASYLAB (light source DORIS III), DESY, Hamburg. An intermediate, Ca(OH)(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3}){center_dot}2H{sub 2}O (2), was observed and could be isolated from the reaction mixture at ambientmore » temperatures by quenching the reaction. The crystal structure of 2 was determined from XRPD data using synchrotron radiation (monoclinic, P2{sub 1}/m, a=11.2193(7), b=7.1488(3), c=5.0635(2) A, {beta}=100.13(4) Degree-Sign , V=399.78(3) A{sup 3}, Z=2). - Graphical abstarct: The detailed in situ energy dispersive X-ray diffraction (EDXRD) investigation on the formation of the new inorganic-organic hybrid compound Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) leads to the discovery of a new crystalline intermediate phase. Both crystal structures were elucidated using X-ray powder diffraction data. Highlights: Black-Right-Pointing-Pointer High-throughput investigation led to new metal aminoethylphosphonate Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}). Black-Right-Pointing-Pointer The formation of Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) was followed by in situ EDXRD measurements. Black-Right-Pointing-Pointer The crystalline intermediate Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3})(OH){center_dot}2H{sub 2}O was discovered. Black-Right-Pointing-Pointer Isolation of Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3})(OH){center_dot}2H{sub 2}O was accomplished by quenching experiments. Black-Right-Pointing-Pointer The structures were determined using X-ray powder diffraction data.« less

Pulse generation and preamplification for long pulse beamlines of Orion laser facility.

PubMed

Hillier, David I; Winter, David N; Hopps, Nicholas W

2010-06-01

We describe the pulse generation, shaping, and preamplification system for the nanosecond beamlines of the Orion laser facility. The system generates shaped laser pulses of up to approximately 1 J of 100 ps-5 ns duration with a programmable temporal profile. The laser has a 30th-power supergaussian spatial profile and is diffraction limited. The system is capable of imposing 2D smoothing by spectral dispersion upon the beam, which will produce a nonuniformity of 10% rms at the target.

Wavefront propagation simulations for a UV/soft x-ray beamline: Electron Spectro-Microscopy beamline at NSLS-II

NASA Astrophysics Data System (ADS)

Canestrari, N.; Bisogni, V.; Walter, A.; Zhu, Y.; Dvorak, J.; Vescovo, E.; Chubar, O.

2014-09-01

A "source-to-sample" wavefront propagation analysis of the Electron Spectro-Microscopy (ESM) UV / soft X-ray beamline, which is under construction at the National Synchrotron Light Source II (NSLS-II) in the Brookhaven National Laboratory, has been conducted. All elements of the beamline - insertion device, mirrors, variable-line-spacing gratings and slits - are included in the simulations. Radiation intensity distributions at the sample position are displayed for representative photon energies in the UV range (20 - 100 eV) where diffraction effects are strong. The finite acceptance of the refocusing mirrors is the dominating factor limiting the spatial resolution at the sample (by ~3 μm at 20 eV). Absolute estimates of the radiation flux and energy resolution at the sample are also obtained from the electromagnetic calculations. The analysis of the propagated UV range undulator radiation at different deflection parameter values demonstrates that within the beamline angular acceptance a slightly "red-shifted" radiation provides higher flux at the sample and better energy resolution compared to the on-axis resonant radiation of the fundamental harmonic.

Optical Tweezers for Sample Fixing in Micro-Diffraction Experiments

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

Amenitsch, H.; Rappolt, M.; Sartori, B.

2007-01-19

In order to manipulate, characterize and measure the micro-diffraction of individual structural elements down to single phospholipid liposomes we have been using optical tweezers (OT) combined with an imaging microscope. We were able to install the OT system at the microfocus beamline ID13 at the ESRF and trap clusters of about 50 multi-lamellar liposomes (< 10 {mu}m large cluster). Further we have performed a scanning diffraction experiment with a 1 micrometer beam to demonstrate the fixing capabilities and to confirm the size of the liposome cluster by X-ray diffraction.

Micro- and nano-tomography at the DIAMOND beamline I13L imaging and coherence

NASA Astrophysics Data System (ADS)

Rau, C.; Bodey, A.; Storm, M.; Cipiccia, S.; Marathe, S.; Zdora, M.-C.; Zanette, I.; Wagner, U.; Batey, D.; Shi, X.

2017-10-01

The Diamond Beamline I13L is dedicated to imaging on the micro- and nano-lengthsale, operating in the energy range between 6 and 30keV. For this purpose two independently operating branchlines and endstations have been built. The imaging branch is fully operational for micro-tomography and in-line phase contrast imaging with micrometre resolution. Grating interferometry is currently implemented, adding the capability of measuring phase and small-angle information. For tomography with increased resolution a full-field microscope providing 50nm spatial resolution with a field of view of 100μm is being tested. The instrument provides a large working distance between optics and sample to adapt a wide range of customised sample environments. On the coherence branch coherent diffraction imaging techniques such as ptychography, coherent X-ray diffraction (CXRD) are currently developed for three dimensional imaging with the highest resolution. The imaging branch is operated in collaboration with Manchester University, called therefore the Diamond-Manchester Branchline. The scientific applications cover a large area including bio-medicine, materials science, chemistry geology and more. The present paper provides an overview about the current status of the beamline and the science addressed.

The Powder Diffraction File: Past, Present, and Future

PubMed Central

Smith, Deane K.; Jenkins, Ron

1996-01-01

The Powder Diffraction file has been the primary reference for Powder Diffraction Data for more than half a century. The file is a collection of about 65 000 reduced powder patterns stored as sets of d/I data along with the appropriate crystallographic, physical and experimental information. This paper reviews the development and growth of the PDF and discusses the role of the ICDD in the maintenance and dissemination of the file. PMID:27805163

Determination of cellulose crystallinity from powder diffraction diagrams: Powder Diffraction Diagrams

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

Lindner, Benjamin; Petridis, Loukas; Langan, Paul

2014-10-01

Commonly one-dimensional (1D) (spherically averaged) powder diffraction diagrams are used to determine the degree of cellulose crystallinity in biomass samples. Here, it is shown using molecular modeling how disorder in cellulose fibrils can lead to considerable uncertainty in conclusions drawn concerning crystallinity based on 1D powder diffraction data alone. For example, cellulose microfibrils that contain both crystalline and noncrystalline segments can lead to powder diffraction diagrams lacking identifiable peaks, while microfibrils without any crystalline segments can lead to such peaks. Moreover, this leads to false positives, that is, assigning disordered cellulose as crystalline, and false negatives, that is, categorizing fibrilsmore » with crystalline segments as amorphous. Finally, the reliable determination of the fraction of crystallinity in any given biomass sample will require a more sophisticated approach combining detailed experiment and simulation.« less

A hybrid method for X-ray optics simulation: combining geometric ray-tracing and wavefront propagation

DOE PAGES

Shi, Xianbo; Reininger, Ruben; Sanchez del Rio, Manuel; ...

2014-05-15

A new method for beamline simulation combining ray-tracing and wavefront propagation is described. The 'Hybrid Method' computes diffraction effects when the beam is clipped by an aperture or mirror length and can also simulate the effect of figure errors in the optical elements when diffraction is present. The effect of different spatial frequencies of figure errors on the image is compared withSHADOWresults pointing to the limitations of the latter. The code has been benchmarked against the multi-electron version ofSRWin one dimension to show its validity in the case of fully, partially and non-coherent beams. The results demonstrate that the codemore » is considerably faster than the multi-electron version ofSRWand is therefore a useful tool for beamline design and optimization.« less

Low-dose, high-resolution and high-efficiency ptychography at STXM beamline of SSRF

NASA Astrophysics Data System (ADS)

Xu, Zijian; Wang, Chunpeng; Liu, Haigang; Tao, Xulei; Tai, Renzhong

2017-06-01

Ptychography is a diffraction-based X-ray microscopy method that can image extended samples quantitatively while remove the resolution limit imposed by image-forming optical elements. As a natural extension of scanning transmission X-ray microscopy (STXM) imaging method, we developed soft X-ray ptychographic coherent diffraction imaging (PCDI) method at the STXM endstation of BL08U beamline of Shanghai Synchrotron Radiation Facility. Compared to the traditional STXM imaging, the new PCDI method has resulted in significantly lower dose, higher resolution and higher efficiency imaging in our platform. In the demonstration experiments shown here, a spatial resolution of sub-10 nm was obtained for a gold nanowires sample, which is much better than the limit resolution 30 nm of the STXM method, while the radiation dose is only 1/12 of STXM.

Development of sample exchange robot PAM-HC for beamline BL-1A at the photon factory

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

Hiraki, Masahiko, E-mail: masahiko.hiraki@kek.jp; Department of Accelerator Science, SOKENDAI; Matsugaki, Naohiro

A macromolecular crystallography beamline, BL-1A, has been built at the Photon Factory (PF) for low energy experiments and has been operational since 2010. We have installed a sample exchange robot, PAM (PF Automated Mounting system), similar to other macromolecular crystallography beamlines. However, following the installation of a helium chamber to reduce the absorption of the diffraction signal by air, we developed a new sample exchange robot to replace PAM. The new robot, named PAM-HC (Helium Chamber), is designed with the goal of minimizing leakage of helium gas from the chamber. Here, the PAM-HC hardware and the flow of its movementmore » are described. Furthermore, measurements of temperature changes during sample exchange are presented in this paper.« less

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

NASA Astrophysics Data System (ADS)

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

1996-09-01

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

Fast helicity switching of x-ray circular polarization at beamline P09 at PETRA III

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

Strempfer, J., E-mail: Joerg.Strempfer@desy.de; Mardegan, J. R. L.; Francoual, S.

At the resonant scattering and diffraction beamline P09 at PETRA III/DESY, polarization manipulation in the X-ray energy range 3-13 keV is possible using wave-plates. Recently, fast flipping of circular polarization helicity using the Raspberry Pi controlled FPGA (PiLC) device developed at DESY and dedicated piezo-electric flippers has been commissioned. Functionality of the PiLC for XMCD and first XMCD measurements at the Fe K-and Dy-L{sub 3} absorption edges are presented.

Symposium LL: Nanowires--Synthesis Properties Assembly and Application

DTIC Science & Technology

2010-09-10

dedicated hard x - ray microscopy beamline is operated in partnership with the Advanced Photon Source to provide fluorescence, diffraction, and...characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X - ray diffraction (XRD) measurements, proving it to be...Investigation of Preferred Growth Direction of GaN Nanorods by Synchrotron X - ray Reciprocal Space Mapping. Yuri Sohn1, Sanghwa Lee1, Chinkyo Kim1 and Dong

Crystallization and preliminary X-ray diffraction analysis of mouse 3(17)α-hydroxysteroid dehydrogenase

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

El-Kabbani, Ossama, E-mail: ossama.el-kabbani@vcp.monash.edu.au; Ishikura, Syuhei; Wagner, Armin

2005-07-01

Orthorhombic crystals of mouse 3(17)α-hydroxysteroid dehydrogenase were obtained from buffered polyethylene glycol solutions. The crystals diffracted to a resolution of 1.8 Å at the Swiss Light Source beamline X06SA. The 3(17)α-hydroxysteroid dehydrogenase from mouse is involved in the metabolism of oestrogens, androgens, neurosteroids and xenobiotic compounds. The enzyme was crystallized by the hanging-drop vapour-diffusion method in space group P222{sub 1}, with unit-cell parameters a = 84.91, b = 84.90, c = 95.83 Å. The Matthews coefficient (V{sub M}) and the solvent content were 2.21 Å{sup 3} Da{sup −1} and 44.6%, respectively, assuming the presence of two molecules in the asymmetricmore » unit. Diffraction data were collected to a resolution of 1.8 Å at the Swiss Light Source beamline X06SA using a MAR CCD area detector and gave a data set with an overall R{sub merge} of 6.8% and a completeness of 91.1%.« less

Main functions, recent updates, and applications of Synchrotron Radiation Workshop code

NASA Astrophysics Data System (ADS)

Chubar, Oleg; Rakitin, Maksim; Chen-Wiegart, Yu-Chen Karen; Chu, Yong S.; Fluerasu, Andrei; Hidas, Dean; Wiegart, Lutz

2017-08-01

The paper presents an overview of the main functions and new application examples of the "Synchrotron Radiation Workshop" (SRW) code. SRW supports high-accuracy calculations of different types of synchrotron radiation, and simulations of propagation of fully-coherent radiation wavefronts, partially-coherent radiation from a finite-emittance electron beam of a storage ring source, and time-/frequency-dependent radiation pulses of a free-electron laser, through X-ray optical elements of a beamline. An extended library of physical-optics "propagators" for different types of reflective, refractive and diffractive X-ray optics with its typical imperfections, implemented in SRW, enable simulation of practically any X-ray beamline in a modern light source facility. The high accuracy of calculation methods used in SRW allows for multiple applications of this code, not only in the area of development of instruments and beamlines for new light source facilities, but also in areas such as electron beam diagnostics, commissioning and performance benchmarking of insertion devices and individual X-ray optical elements of beamlines. Applications of SRW in these areas, facilitating development and advanced commissioning of beamlines at the National Synchrotron Light Source II (NSLS-II), are described.

The protein crystallography beamline at LNLS, the Brazilian National Synchrotron Light Source

NASA Astrophysics Data System (ADS)

Polikarpov, I.; Oliva, G.; Castellano, E. E.; Garratt, R. C.; Arruda, P.; Leite, A.; Craievich, A.

1998-02-01

The Brazilian National Synchrotron Light Laboratory - LNLS, will have a dedicated protein crystallography beamline. The beamline under construction includes cylindrical mirror and bent crystal monochromator focusing the high flux of synchrotron radiation in the horizontal plane at the position of the sample. The monochromatic radiation will be tuneable between 2.0 and 1.0 Å with the optimum wavelength at 1.3-1.6 Å, chosen with the aim of maximizing the photon flux from the bending magnets of the storage ring (1.37 GeV). Diffraction images will be recorded on a commercial image plate detector system with on-line readout. The beamline set-up will include cooler/chiller for the samples and biochemical lab for crystallization, heavy-metal soaks, crystal storage and mounting at 22°C and 4°C, will also be available. The facility, intended to serve the national and international community, is planned to be brought into operation in the second half of 1997. It is foreseen that the commissioning of the first protein crystallography beamline in Latin America will boost the number of protein structures determined locally and will increase the general interest of the molecular biology and biochemical research community of Brazil in this area.

JCPDS-ICDD Research Associateship (Cooperative Program with NBS/NIST)

PubMed Central

Wong-Ng, W.; McMurdie, H. F.; Hubbard, C. R.; Mighell, A. D.

2001-01-01

The Research Associateship program of the Joint Committee on Powder Diffraction-International Centre for Diffraction Data (JCPDS-ICDD, now known as the ICDD) at NBS/NIST was a long standing (over 35 years) successful industry-government cooperation. The main mission of the Associateship was to publish high quality x-ray reference patterns to be included in the Powder Diffraction File (PDF). The PDF is a continuing compilation of patterns gathered from many sources, compiled and published by the ICDD. As a result of this collaboration, more than 1500 high quality powder diffraction patterns, which have had a significant impact on the scientific community, were reported. In addition, various research collaborations with NBS/NIST also led to the development of several standard reference materials (SRMs) for instrument calibration and quantitative analyses, and computer software for data collection, calibration, reduction, for the editorial process of powder pattern publication, analysis of powder data, and for quantitative analyses. This article summarizes information concerning the JCPDS-ICDD organization, the Powder Diffraction File (PDF), history and accomplishments of the JCPDS-ICDD Research Associateship. PMID:27500061

Fast two-dimensional grid and transmission X-ray microscopy scanning methods for visualizing and characterizing protein crystals

PubMed Central

Wojdyla, Justyna Aleksandra; Panepucci, Ezequiel; Martiel, Isabelle; Ebner, Simon; Huang, Chia-Ying; Caffrey, Martin; Bunk, Oliver; Wang, Meitian

2016-01-01

A fast continuous grid scan protocol has been incorporated into the Swiss Light Source (SLS) data acquisition and analysis software suite on the macromolecular crystallography (MX) beamlines. Its combination with fast readout single-photon counting hybrid pixel array detectors (PILATUS and EIGER) allows for diffraction-based identification of crystal diffraction hotspots and the location and centering of membrane protein microcrystals in the lipid cubic phase (LCP) in in meso in situ serial crystallography plates and silicon nitride supports. Diffraction-based continuous grid scans with both still and oscillation images are supported. Examples that include a grid scan of a large (50 nl) LCP bolus and analysis of the resulting diffraction images are presented. Scanning transmission X-ray microscopy (STXM) complements and benefits from fast grid scanning. STXM has been demonstrated at the SLS beamline X06SA for near-zero-dose detection of protein crystals mounted on different types of sample supports at room and cryogenic temperatures. Flash-cooled crystals in nylon loops were successfully identified in differential and integrated phase images. Crystals of just 10 µm thickness were visible in integrated phase images using data collected with the EIGER detector. STXM offers a truly low-dose method for locating crystals on solid supports prior to diffraction data collection at both synchrotron microfocusing and free-electron laser X-ray facilities. PMID:27275141

Linking structural biology with genome research: Beamlines for the Berlin ``Protein Structure Factory'' initiative

NASA Astrophysics Data System (ADS)

Illing, Gerd; Saenger, Wolfram; Heinemann, Udo

2000-06-01

The Protein Structure Factory will be established to characterize proteins encoded by human genes or cDNAs, which will be selected by criteria of potential structural novelty or medical or biotechnological usefulness. It represents an integrative approach to structure analysis combining bioinformatics techniques, automated gene expression and purification of gene products, generation of a biophysical fingerprint of the proteins and the determination of their three-dimensional structures either by NMR spectroscopy or by X-ray diffraction. The use of synchrotron radiation will be crucial to the Protein Structure Factory: high brilliance and tunable wavelengths are prerequisites for fast data collection, the use of small crystals and multiwavelength anomalous diffraction (MAD) phasing. With the opening of BESSY II, direct access to a third-generation XUV storage ring source with excellent conditions is available nearby. An insertion device with two MAD beamlines and one constant energy station will be set up until 2001.

Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography

PubMed Central

Mueller, C.; Marx, A.; Epp, S. W.; Zhong, Y.; Kuo, A.; Balo, A. R.; Soman, J.; Schotte, F.; Lemke, H. T.; Owen, R. L.; Pai, E. F.; Pearson, A. R.; Olson, J. S.; Anfinrud, P. A.; Ernst, O. P.; Dwayne Miller, R. J.

2015-01-01

We present a crystallography chip enabling in situ room temperature crystallography at microfocus synchrotron beamlines and X-ray free-electron laser (X-FEL) sources. Compared to other in situ approaches, we observe extremely low background and high diffraction data quality. The chip design is robust and allows fast and efficient loading of thousands of small crystals. The ability to load a large number of protein crystals, at room temperature and with high efficiency, into prescribed positions enables high throughput automated serial crystallography with microfocus synchrotron beamlines. In addition, we demonstrate the application of this chip for femtosecond time-resolved serial crystallography at the Linac Coherent Light Source (LCLS, Menlo Park, California, USA). The chip concept enables multiple images to be acquired from each crystal, allowing differential detection of changes in diffraction intensities in order to obtain high signal-to-noise and fully exploit the time resolution capabilities of XFELs. PMID:26798825

Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography.

PubMed

Mueller, C; Marx, A; Epp, S W; Zhong, Y; Kuo, A; Balo, A R; Soman, J; Schotte, F; Lemke, H T; Owen, R L; Pai, E F; Pearson, A R; Olson, J S; Anfinrud, P A; Ernst, O P; Dwayne Miller, R J

2015-09-01

We present a crystallography chip enabling in situ room temperature crystallography at microfocus synchrotron beamlines and X-ray free-electron laser (X-FEL) sources. Compared to other in situ approaches, we observe extremely low background and high diffraction data quality. The chip design is robust and allows fast and efficient loading of thousands of small crystals. The ability to load a large number of protein crystals, at room temperature and with high efficiency, into prescribed positions enables high throughput automated serial crystallography with microfocus synchrotron beamlines. In addition, we demonstrate the application of this chip for femtosecond time-resolved serial crystallography at the Linac Coherent Light Source (LCLS, Menlo Park, California, USA). The chip concept enables multiple images to be acquired from each crystal, allowing differential detection of changes in diffraction intensities in order to obtain high signal-to-noise and fully exploit the time resolution capabilities of XFELs.

Development of at-wavelength metrology for x-ray optics at the ALS

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

Yashchuk, Valeriy V.; Goldberg, Kenneth A.; Yuan, Sheng

2010-07-09

The comprehensive realization of the exciting advantages of new third- and forth-generation synchrotron radiation light sources requires concomitant development of reflecting and diffractive x-ray optics capable of micro- and nano-focusing, brightness preservation, and super high resolution. The fabrication, tuning, and alignment of the optics are impossible without adequate metrology instrumentation, methods, and techniques. While the accuracy of ex situ optical metrology at the Advanced Light Source (ALS) has reached a state-of-the-art level, wavefront control on beamlines is often limited by environmental and systematic alignment factors, and inadequate in situ feedback. At ALS beamline 5.3.1, we are developing broadly applicable, high-accuracy,more » in situ, at-wavelength wavefront measurement techniques to surpass 100-nrad slope measurement accuracy for Kirkpatrick-Baez (KB) mirrors. The at-wavelength methodology we are developing relies on a series of tests with increasing accuracy and sensitivity. Geometric Hartmann tests, performed with a scanning illuminated sub-aperture determine the wavefront slope across the full mirror aperture. Shearing interferometry techniques use coherent illumination and provide higher sensitivity wavefront measurements. Combining these techniques with high precision optical metrology and experimental methods will enable us to provide in situ setting and alignment of bendable x-ray optics to realize diffraction-limited, sub 50 nm focusing at beamlines. We describe here details of the metrology beamline endstation, the x-ray beam diagnostic system, and original experimental techniques that have already allowed us to precisely set a bendable KB mirror to achieve a focused spot size of 150 nm.« less

Toyota beamline (BL33XU) at SPring-8

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

Nonaka, T., E-mail: nonaka@mosk.tytlabs.co.jp; Dohmae, K.; Hayashi, Y.

2016-07-27

The Toyota beamline (BL33XU) at SPring-8 is an undulator beamline developed to assist in the study of various automotive-related materials. The light source is a tapered in-vacuum undulator that provides a variable energy band width as well as a high brilliance X-ray beam. Two different optical arrangements are available: Optics 1 and Optics 2. Optics 1 is dedicated to time-resolved X-ray absorption spectroscopy (XAFS), and consists of two channel-cut crystal monochromators and four water-cooled flat Si mirrors. The Si(111) and Si(220) monochromator crystals cover an energy range of 4.0–46.0 keV and are driven by high-speed AC servo motors. These monochromators,more » in conjunction with the tapered undulator, enable high-quality XAFS data acquisition with a temporal resolution of 10 ms. Optics 2 is optimized for X-ray diffraction, scattering and imaging and includes a recently installed double crystal monochromator, two water-cooled flat Si mirrors and Kirkpatrick-Baez (KB) focusing mirrors. The monochromator incorporates parallel mounted Si(111) and Si(311) crystals and covers an energy range of 4.5–70 keV. The beamline provides two experimental stations: Exp. Hutch 2 and Exp. Hutch 3. The gas supply system and mass spectrometers installed in Exp. Hutch 2 allow in-operando measurements under various atmospheres. The scanning three-dimensional X-ray diffraction (scanning 3DXRD) microscopy instrumentation developed and installed in Exp. Hutch 3 enables non-destructive orientation and stress mapping of 1 mm-thick steel specimens using a high energy microbeam.« less

Total-scattering pair-distribution function of organic material from powder electron diffraction data.

PubMed

Gorelik, Tatiana E; Schmidt, Martin U; Kolb, Ute; Billinge, Simon J L

2015-04-01

This paper shows that pair-distribution function (PDF) analyses can be carried out on organic and organometallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction and nanodiffraction in transmission electron microscopy or nanodiffraction in scanning transmission electron microscopy modes. The methods were demonstrated on organometallic complexes (chlorinated and unchlorinated copper phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering data and avoiding beam damage of the sample are possible to resolve.

Crystal Structure of 17α-Dihydroequilin, C18H22O2, from Synchrotron Powder Diffraction Data and Density Functional Theory

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

Kaduk, James; Gindhart, Amy; Blanton, Thomas

The crystal structure of 17α-dihydroequilin has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. 17α-dihydroequilin crystallizes in space group P212121 (#19) with a = 6.76849(1) Å, b = 8.96849(1) Å, c = 23.39031(5) Å, V = 1419.915(3) Å3, and Z = 4. Both hydroxyl groups form hydrogen bonds to each other, resulting in zig-zag chains along the b-axis. The powder diffraction pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ as the entry 00-066-1608.

New Powder Diffraction File (PDF-4) in relational database format: advantages and data-mining capabilities.

PubMed

Kabekkodu, Soorya N; Faber, John; Fawcett, Tim

2002-06-01

The International Centre for Diffraction Data (ICDD) is responding to the changing needs in powder diffraction and materials analysis by developing the Powder Diffraction File (PDF) in a very flexible relational database (RDB) format. The PDF now contains 136,895 powder diffraction patterns. In this paper, an attempt is made to give an overview of the PDF-4, search/match methods and the advantages of having the PDF-4 in RDB format. Some case studies have been carried out to search for crystallization trends, properties, frequencies of space groups and prototype structures. These studies give a good understanding of the basic structural aspects of classes of compounds present in the database. The present paper also reports data-mining techniques and demonstrates the power of a relational database over the traditional (flat-file) database structures.

Neutron and X-ray diffraction of plasma-sprayed zirconia-yttria thermal barrier coatings

NASA Technical Reports Server (NTRS)

Shankar, N. R.; Herman, H.; Singhal, S. P.; Berndt, C. C.

1984-01-01

ZrO2-7.8mol. pct. YO1.5, a fused powder, and ZrO2-8.7mol. pct. YO1.5, a prereacted powder, were plasma-sprayed onto steel substrates. Neutron diffraction and X-ray diffraction of the as-received powder, the powder plasma sprayed into water, as-sprayed coatings, and coatings heat-treated for 10 and 100 h were carried out to study phase transformations and ordering of the oxygen ions on the oxygen sublattice. The as-received fused powder has a much lower monoclinic percentage than does the pre-reacted powder, this resulting in a much lower monoclinic percentage in the coating. Heat treatment increases the percentages of the cubic and monoclinic phases, while decreasing the tetragonal content. An ordered tetragonal phase is detected by the presence of extra neutron diffraction peaks. These phase transformations and ordering will result in volume changes. The implications of these transformations on the performance of partially stabilized zirconia thermal barrier coatings is discussed.

High-throughput continuous hydrothermal synthesis of an entire nanoceramic phase diagram.

PubMed

Weng, Xiaole; Cockcroft, Jeremy K; Hyett, Geoffrey; Vickers, Martin; Boldrin, Paul; Tang, Chiu C; Thompson, Stephen P; Parker, Julia E; Knowles, Jonathan C; Rehman, Ihtesham; Parkin, Ivan; Evans, Julian R G; Darr, Jawwad A

2009-01-01

A novel High-Throughput Continuous Hydrothermal (HiTCH) flow synthesis reactor was used to make directly and rapidly a 66-sample nanoparticle library (entire phase diagram) of nanocrystalline Ce(x)Zr(y)Y(z)O(2-delta) in less than 12 h. High resolution PXRD data were obtained for the entire heat-treated library (at 1000 degrees C/1 h) in less than a day using the new robotic beamline I11, located at Diamond Light Source (DLS). This allowed Rietveld-quality powder X-ray diffraction (PXRD) data collection of the entire 66-sample library in <1 day. Consequently, the authors rapidly mapped out phase behavior and sintering behaviors for the entire library. Out of the entire 66-sample heat-treated library, the PXRD data suggests that 43 possess the fluorite structure, of which 30 (out of 36) are ternary compositions. The speed, quantity and quality of data obtained by our new approach, offers an exciting new development which will allow structure-property relationships to be accessed for nanoceramics in much shorter time periods.

Nm-scale spatial resolution x-ray imaging with MLL nanofocusing optics: instrumentational requirements and challenges

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

Nazaretski, E.; Yan, H.; Lauer, K.

2016-08-30

The Hard X-ray Nanoprobe (HXN) beamline at NSLS-II has been designed and constructed to enable imaging experiments with unprecedented spatial resolution and detection sensitivity. The HXN X-ray Microscope is a key instrument for the beamline, providing a suite of experimental capabilities which includes scanning fluorescence, diffraction, differential phase contrast and ptychography utilizing Multilayer Laue Lenses (MLL) and zoneplate (ZP) as nanofocusing optics. In this paper, we present technical requirements for the MLL-based scanning microscope, outline the development concept and present first ~15 x 15 nm 2 spatial resolution x-ray fluorescence images.

Total-scattering pair-distribution function of organic material from powder electron diffraction data

DOE PAGES

Gorelik, Tatiana E.; Billinge, Simon J. L.; Schmidt, Martin U.; ...

2015-04-01

This paper shows for the first time that pair-distribution function analyses can be carried out on organic and organo-metallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction (SAED) and nanodiffraction in transmission electron microscopy (TEM) or nanodiffraction in scanning transmission electron microscopy (STEM) modes. The methods were demonstrated on organo-metallic complexes (chlorinated and unchlorinated copper-phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering datamore » and avoiding beam-damage of the sample are possible to resolve.« less

The HB-2D Polarized Neutron Development Beamline at the High Flux Isotope Reactor

NASA Astrophysics Data System (ADS)

Crow, Lowell; Hamilton, WA; Zhao, JK; Robertson, JL

2016-09-01

The Polarized Neutron Development beamline, recently commissioned at the HB-2D position on the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory, provides a tool for development and testing of polarizers, polarized neutron devices, and prototyping of polarized neutron techniques. With available monochromators including pyrolytic graphite and polarizing enriched Fe-57 (Si), the instrument has operated at 4.25 and 2.6 Å wavelengths, using crystal, supermirror, or He-3 polarizers and analyzers in various configurations. The Neutron Optics and Development Team has used the beamline for testing of He-3 polarizers for use at other HFIR and Spallation Neutron Source (SNS) instruments, as well as a variety of flipper devices. Recently, we have acquired new supermirror polarizers which have improved the instrument performance. The team and collaborators also have continuing demonstration experiments of spin-echo focusing techniques, and plans to conduct polarized diffraction measurements. The beamline is also used to support a growing use of polarization techniques at present and future instruments at SNS and HFIR.

Characterization of the X-ray coherence properties of an undulator beamline at the Advanced Photon Source

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

Ju, Guangxu; Highland, Matthew J.; Thompson, Carol

In anticipation of the increased use of coherent X-ray methods and the need to upgrade beamlines to match improved source quality, here the coherence properties of the X-rays delivered by beamline 12ID-D at the Advanced Photon Source have been characterized. The measured X-ray divergence, beam size, brightness and coherent flux at energies up to 26 keV are compared with the calculated values from the undulator source, and the effects of beamline optics such as a mirror, monochromator and compound refractive lenses are evaluated. Diffraction patterns from slits as a function of slit width are analyzed using wave propagation theory tomore » obtain the beam divergence and thus coherence length. Imaging of the source using a compound refractive lens was found to be the most accurate method for determining the vertical divergence. While the brightness and coherent flux obtained without a monochromator ('pink beam') agree well with those calculated for the source, those measured with the monochromator were a factor of three to six lower than the source, primarily because of vertical divergence introduced by the monochromator. As a result, the methods described herein should be widely applicable for measuring the X-ray coherence properties of synchrotron beamlines.« less

Characterization of the X-ray coherence properties of an undulator beamline at the Advanced Photon Source

DOE PAGES

Ju, Guangxu; Highland, Matthew J.; Thompson, Carol; ...

2018-06-13

In anticipation of the increased use of coherent X-ray methods and the need to upgrade beamlines to match improved source quality, here the coherence properties of the X-rays delivered by beamline 12ID-D at the Advanced Photon Source have been characterized. The measured X-ray divergence, beam size, brightness and coherent flux at energies up to 26 keV are compared with the calculated values from the undulator source, and the effects of beamline optics such as a mirror, monochromator and compound refractive lenses are evaluated. Diffraction patterns from slits as a function of slit width are analyzed using wave propagation theory tomore » obtain the beam divergence and thus coherence length. Imaging of the source using a compound refractive lens was found to be the most accurate method for determining the vertical divergence. While the brightness and coherent flux obtained without a monochromator ('pink beam') agree well with those calculated for the source, those measured with the monochromator were a factor of three to six lower than the source, primarily because of vertical divergence introduced by the monochromator. As a result, the methods described herein should be widely applicable for measuring the X-ray coherence properties of synchrotron beamlines.« less

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

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig 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

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

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

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

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

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

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 (<2µl) 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 tomore » 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 (10–15µm) loaded into the chips yielded a complete, high-resolution (<1.6Å) data set sufficient to determine a high-quality structure by molecular replacement. 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

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

PubMed Central

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

2015-01-01

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 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 (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. 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. PMID:26457423

Metrology of variable-line-spacing x-ray gratings using the APS Long Trace Profiler

NASA Astrophysics Data System (ADS)

Sheung, Janet; Qian, Jun; Sullivan, Joseph; Thomasset, Muriel; Manton, Jonathan; Bean, Sunil; Takacs, Peter; Dvorak, Joseph; Assoufid, Lahsen

2017-09-01

As resolving power targets have increased with each generation of beamlines commissioned in synchrotron radiation facilities worldwide, diffraction gratings are quickly becoming crucial optical components for meeting performance targets. However, the metrology of variable-line-spacing (VLS) gratings for high resolution beamlines is not widespread; in particular, no metrology facility at any US DOE facility is currently equipped to fully characterize such gratings. To begin to address this issue, the Optics Group at the Advanced Photon Source at Argonne, in collaboration with SOLEIL and with support from Brookhaven National Laboratory (BNL), has developed an alternative beam path addition to the Long Trace Profiler (LTP) at Argonne's Advanced Photon Source. This significantly expands the functionality of the LTP not only to measure mirrors surface slope profile at normal incidence, but also to characterize the groove density of VLS diffraction gratings in the Littrow incidence up to 79°, which covers virtually all diffraction gratings used at synchrotrons in the first order. The LTP light source is a 20mW HeNe laser, which yields enough signal for diffraction measurements to be performed on low angle blazed gratings optimized for soft X-ray wavelengths. We will present the design of the beam path, technical requirements for the optomechanics, and our data analysis procedure. Finally, we discuss challenges still to be overcome and potential limitations with use of the LTP to perform metrology on diffraction gratings.

Interoperability and complementarity of simulation tools for beamline design in the OASYS environment

NASA Astrophysics Data System (ADS)

Rebuffi, Luca; Sanchez del Rio, Manuel

2017-08-01

In the next years most of the major synchrotron radiation facilities around the world will upgrade to 4th-generation Diffraction Limited Storage Rings using multi-bend-achromat technology. Moreover, several Free Electron Lasers are ready-to-go or in phase of completion. These events represent a huge challenge for the optics physicists responsible of designing and calculating optical systems capable to exploit the revolutionary characteristics of the new photon beams. Reliable and robust beamline design is nowadays based on sophisticated computer simulations only possible by lumping together different simulation tools. The OASYS (OrAnge SYnchrotron Suite) suite drives several simulation tools providing new mechanisms of interoperability and communication within the same software environment. OASYS has been successfully used during the conceptual design of many beamline and optical designs for the ESRF and Elettra- Sincrotrone Trieste upgrades. Some examples are presented showing comparisons and benchmarking of simulations against calculated and experimental data.

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

Flechsig, U.; Follath, R.; Reiche, S.

PHASE is a software tool for physical optics simulation based on the stationary phase approximation method. The code is under continuous development since about 20 years and has been used for instance for fundamental studies and ray tracing of various beamlines at the Swiss Light Source. Along with the planning for SwissFEL a new hard X-ray free electron laser under construction, new features have been added to permit practical performance predictions including diffraction effects which emerge with the fully coherent source. We present the application of the package on the example of the ARAMIS 1 beamline at SwissFEL. The X-raymore » pulse calculated with GENESIS and given as an electrical field distribution has been propagated through the beamline to the sample position. We demonstrate the new features of PHASE like the treatment of measured figure errors, apertures and coatings of the mirrors and the application of Fourier optics propagators for free space propagation.« less

Optical design and simulation of a new coherence beamline at NSLS-II

NASA Astrophysics Data System (ADS)

Williams, Garth J.; Chubar, Oleg; Berman, Lonny; Chu, Yong S.; Robinson, Ian K.

2017-08-01

We will discuss the optical design for a proposed beamline at NSLS-II, a late-third generation storage ring source, designed to exploit the spatial coherence of the X-rays to extract high-resolution spatial information from ordered and disordered materials through Coherent Diffractive Imaging, executed in the Bragg- and forward-scattering geometries. This technique offers a powerful tool to image sub-10 nm spatial features and, within ordered materials, sub-Angstrom mapping of deformation fields. Driven by the opportunity to apply CDI to a wide range of samples, with sizes ranging from sub-micron to tens-of-microns, two optical designs have been proposed and simulated under a wide variety of optical configurations using the software package Synchrotron Radiation Workshop. The designs, their goals, and the results of the simulation, including NSLS-II ring and undulator source parameters, of the beamline performance as a function of its variable optical components is described.

Nanofiber-Based Bulk-Heterojunction Organic Solar Cells Using Coaxial Electrospinning

DTIC Science & Technology

2012-01-01

chains are likely oriented with the [010] direction, perpendicular to the substrate, in the fi lm device. Glancing incidence X - ray diffraction (GIXD...Electron and X - ray diffraction measurements were per- formed in order to study the structural order in annealed fi bers and devices. For reference... angle X - ray scattering (SAXS/WAXS) beamline 7.3.3 of the Advanced Light Source at Lawrence Berkeley National Laboratory at 10 keV (1.24 Å) from a bend

Simultaneous X-ray fluorescence and scanning X-ray diffraction microscopy at the Australian Synchrotron XFM beamline

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

Jones, Michael W. M.; Phillips, Nicholas W.; van Riessen, Grant A.

2016-08-11

Owing to its extreme sensitivity, quantitative mapping of elemental distributionsviaX-ray fluorescence microscopy (XFM) has become a key microanalytical technique. The recent realisation of scanning X-ray diffraction microscopy (SXDM) meanwhile provides an avenue for quantitative super-resolved ultra-structural visualization. The similarity of their experimental geometries indicates excellent prospects for simultaneous acquisition. Here, in both step- and fly-scanning modes, robust, simultaneous XFM-SXDM is demonstrated.

Crystallization and X-ray diffraction analysis of a catalytic domain of hyperthermophilic chitinase from Pyrococcus furiosus

PubMed Central

Mine, Shouhei; Nakamura, Tsutomu; Hirata, Kunio; Ishikawa, Kazuhiko; Hagihara, Yoshihisa; Uegaki, Koichi

2006-01-01

The crystallization and preliminary X-ray diffraction analysis of a catalytic domain of chitinase (PF1233 gene) from the hyperthermophilic archaeon Pyrococcus furiosus is reported. The recombinant protein, prepared using an Escherichia coli expression system, was crystallized by the hanging-drop vapour-diffusion method. An X-ray diffraction data set was collected at the undulator beamline BL44XU at SPring-8 to a resolution of 1.50 Å. The crystals belong to space group P212121, with unit-cell parameters a = 90.0, b = 92.8, c = 107.2 Å. PMID:16880559

Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography

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

Mueller, C.; Marx, A.; Epp, S. W.

We present a crystallography chip enabling in situ room temperature crystallography at microfocus synchrotron beamlines and X-ray free-electron laser (X-FEL) sources. Compared to other in situ approaches, we observe extremely low background and high diffraction data quality. The chip design is robust and allows fast and efficient loading of thousands of small crystals. The ability to load a large number of protein crystals, at room temperature and with high efficiency, into prescribed positions enables high throughput automated serial crystallography with microfocus synchrotron beamlines. In addition, we demonstrate the application of this chip for femtosecond time-resolved serial crystallography at the Linacmore » Coherent Light Source (LCLS, Menlo Park, California, USA). As a result, the chip concept enables multiple images to be acquired from each crystal, allowing differential detection of changes in diffraction intensities in order to obtain high signal-to-noise and fully exploit the time resolution capabilities of XFELs.« less

Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography

DOE PAGES

Mueller, C.; Marx, A.; Epp, S. W.; ...

2015-08-18

We present a crystallography chip enabling in situ room temperature crystallography at microfocus synchrotron beamlines and X-ray free-electron laser (X-FEL) sources. Compared to other in situ approaches, we observe extremely low background and high diffraction data quality. The chip design is robust and allows fast and efficient loading of thousands of small crystals. The ability to load a large number of protein crystals, at room temperature and with high efficiency, into prescribed positions enables high throughput automated serial crystallography with microfocus synchrotron beamlines. In addition, we demonstrate the application of this chip for femtosecond time-resolved serial crystallography at the Linacmore » Coherent Light Source (LCLS, Menlo Park, California, USA). As a result, the chip concept enables multiple images to be acquired from each crystal, allowing differential detection of changes in diffraction intensities in order to obtain high signal-to-noise and fully exploit the time resolution capabilities of XFELs.« less

The high-energy x-ray diffraction and scattering beamline at the Canadian Light Source

NASA Astrophysics Data System (ADS)

Gomez, A.; Dina, G.; Kycia, S.

2018-06-01

The optical design for the high-energy x-ray diffraction and scattering beamline of the Brockhouse sector at the Canadian Light Source is described. The design is based on a single side-bounce silicon focusing monochromator that steers the central part of a high-field permanent magnet wiggler beam into the experimental station. Two different configurations are proposed: a higher energy resolution with vertical focusing and a lower energy resolution with horizontal and vertical focusing. The monochromator will have the possibility of mounting three crystals: one crystal optimized for 35 keV that focuses in the horizontal and vertical directions using reflection (1,1,1) and two other crystals both covering the energies above 40 keV: one with only vertical focusing and another one with horizontal and vertical focusing. The geometry of the last two monochromator crystals was optimized to use reflections (4,2,2) and (5,3,3) to cover the broad energy range from 40 to 95 keV.

Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

NASA Astrophysics Data System (ADS)

Tanaka, M.; Katsuya, Y.; Matsushita, Y.

2013-03-01

The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

Scanning force microscope for in situ nanofocused X-ray diffraction studies

PubMed Central

Ren, Zhe; Mastropietro, Francesca; Davydok, Anton; Langlais, Simon; Richard, Marie-Ingrid; Furter, Jean-Jacques; Thomas, Olivier; Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume; Boesecke, Peter; Cornelius, Thomas W.

2014-01-01

A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials. PMID:25178002

A beamline for high-pressure studies at the Advanced Light Source with a superconducting bending magnet as the source.

PubMed

Kunz, Martin; MacDowell, Alastair A; Caldwell, Wendel A; Cambie, Daniella; Celestre, Richard S; Domning, Edward E; Duarte, Robert M; Gleason, Arianna E; Glossinger, James M; Kelez, Nicholas; Plate, David W; Yu, Tony; Zaug, Joeseph M; Padmore, Howard A; Jeanloz, Raymond; Alivisatos, A Paul; Clark, Simon M

2005-09-01

A new facility for high-pressure diffraction and spectroscopy using diamond anvil high-pressure cells has been built at the Advanced Light Source on beamline 12.2.2. This beamline benefits from the hard X-radiation generated by a 6 T superconducting bending magnet (superbend). Useful X-ray flux is available between 5 keV and 35 keV. The radiation is transferred from the superbend to the experimental enclosure by the brightness-preserving optics of the beamline. These optics are comprised of a plane parabola collimating mirror, followed by a Kohzu monochromator vessel with Si(111) crystals (E/DeltaE approximately equal 7000) and W/B4C multilayers (E/DeltaE approximately equal 100), and then a toroidal focusing mirror with variable focusing distance. The experimental enclosure contains an automated beam-positioning system, a set of slits, ion chambers, the sample positioning goniometry and area detector (CCD or image-plate detector). Future developments aim at the installation of a second endstation dedicated to in situ laser heating and a dedicated high-pressure single-crystal station, applying both monochromatic and polychromatic techniques.

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

PubMed Central

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

2016-01-01

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

Expected values and variances of Bragg peak intensities measured in a nanocrystalline powder diffraction experiment

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

Öztürk, Hande; Noyan, I. Cevdet

A rigorous study of sampling and intensity statistics applicable for a powder diffraction experiment as a function of crystallite size is presented. Our analysis yields approximate equations for the expected value, variance and standard deviations for both the number of diffracting grains and the corresponding diffracted intensity for a given Bragg peak. The classical formalism published in 1948 by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] appears as a special case, limited to large crystallite sizes, here. It is observed that both the Lorentz probability expression and the statistics equations used in the classical formalism are inapplicable for nanocrystallinemore » powder samples.« less

Expected values and variances of Bragg peak intensities measured in a nanocrystalline powder diffraction experiment

DOE PAGES

Öztürk, Hande; Noyan, I. Cevdet

2017-08-24

A rigorous study of sampling and intensity statistics applicable for a powder diffraction experiment as a function of crystallite size is presented. Our analysis yields approximate equations for the expected value, variance and standard deviations for both the number of diffracting grains and the corresponding diffracted intensity for a given Bragg peak. The classical formalism published in 1948 by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] appears as a special case, limited to large crystallite sizes, here. It is observed that both the Lorentz probability expression and the statistics equations used in the classical formalism are inapplicable for nanocrystallinemore » powder samples.« less

NSLS-II biomedical beamlines for micro-crystallography, FMX, and for highly automated crystallography, AMX: New opportunities for advanced data collection

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

Fuchs, Martin R., E-mail: mfuchs@bnl.gov; Bhogadi, Dileep K.; Jakoncic, Jean

We present the final design of the x-ray optics and experimental stations of two macromolecular crystallography (MX) beamlines at the National Synchrotron Light Source-II. The microfocusing FMX beamline will deliver a flux of ∼5×10{sup 12} ph/s at 1 Å into a 1 – 20 µm spot, its flux density surpassing current MX beamlines by up to two orders of magnitude. It covers an energy range from 5 – 30 keV. The highly automated AMX beamline is optimized for high throughput, with beam sizes from 4 – 100 µm, an energy range of 5 – 18 keV and a flux atmore » 1 Å of ∼10{sup 13} ph/s. A focus in designing the beamlines lay on achieving high beam stability, for example by implementing a horizontal bounce double crystal monochromator at FMX. A combination of compound refractive lenses and bimorph mirror optics at FMX supports rapid beam size changes. Central components of the in-house developed experimental stations are horizontal axis goniometers with a target sphere of confusion of 100 nm, piezo-slits for dynamic beam size changes during diffraction experiments, dedicated secondary goniometers for data collection from specimen in crystallization plates, and next generation pixel array detectors. FMX and AMX will support a broad range of biomedical structure determination methods from serial crystallography on micron-sized crystals, to structure determination of complexes in large unit cells, to rapid sample screening and room temperature data collection of crystals in trays.« less

Thermal analysis, X-ray powder diffraction and electron microscopy data related with the production of 1:1 Caffeine:Glutaric Acid cocrystals.

PubMed

Duarte, Íris; Andrade, Rita; Pinto, João F; Temtem, Márcio

2016-09-01

The data presented in this article are related to the production of 1:1 Caffeine:Glutaric Acid cocrystals as part of the research article entitled "Green production of cocrystals using a new solvent-free approach by spray congealing" (Duarte et al., 2016) [1]. More specifically, here we present the thermal analysis and the X-ray powder diffraction data for pure Glutaric Acid, used as a raw material in [1]. We also include the X-ray powder diffraction and electron microscopy data obtained for the 1:1 Caffeine:Glutaric Acid cocrystal (form II) produced using the cooling crystallization method reported in "Operating Regions in Cooling Cocrystallization of Caffeine and Glutaric Acid in Acetonitrile" (Yu et al., 2010) [2]. Lastly, we show the X-ray powder diffraction data obtained for assessing the purity of the 1:1 Caffeine:Glutaric cocrystals produced in [1].

Synthesis of nanostructured vanadium powder by high-energy ball milling: X-ray diffraction and high-resolution electron microscopy characterization

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran

2016-10-01

Vanadium metal powders, ball milled with different surfactants viz., stearic acid, KCl and NaCl, have been studied by X-ray diffraction and transmission electron microscopy. The surfactants alter the microstructural and morphological characteristics of the powders. Ball milling with stearic acid results in solid-state amorphization, while powders milled with KCl yield vanadium-tungsten carbide nanocomposite mixtures. NaCl proved to be an excellent surfactant for obtaining nanostructured fusion-grade vanadium powders. In order to understand the reaction mechanism behind any interstitial addition in the ball-milled powders, CHNOS analysis was performed.

Lattice-Preferred Orientation in Deformed Novaculite - Comparison of in-situ Results Using BEARTEX and Post-Mortem EBSD Analyses

NASA Astrophysics Data System (ADS)

Willenweber, A.; Thomas, S.; Burnley, P. C.

2012-12-01

The Berkeley Texture Package BEARTEX is a Windows-based computer software that combines various algorithms to analyze lattice-preferred orientation in polycrystalline materials. BEARTEX was initially designed to interpret diffraction intensity data from pole figure goniometers. Recently it has been successfully used to process synthetic forsterite powder diffraction data from in-situ synchrotron X-ray diffraction taken during deformation (Bollinger et al. 2012). Our study aims to test the practicability of using BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz (novaculite) during deformation. In-situ X-ray diffraction data was collected during the deformation of novaculite at 2.5 GPa and up to 1000 °C in a D-DIA apparatus using the ten-element energy-dispersive detector at the NSLS beamline X17B2. Diffraction intensities are a function of crystal orientation, expressed in azimuth angle η and pole distance ψ. The latter is the angle between the normal of a given diffraction plane and the vertical direction of the D-DIA apparatus - our principal stress direction during compression. Orientation-dependent diffraction intensities were corrected for different responses of the single detectors and x-ray absorption effects of the anvils. Orientation distributions (ODs) and inverse pole figures were calculated using BEARTEX. In addition, electron backscatter diffraction (EBSD) analyses were carried out on the deformed novaculite samples. Generated pole figures were compared with those derived from BEARTEX. Textural properties of our novaculite starting material complicated the BEARTEX analyses. The relatively strong variation of grain sizes in our natural specimens caused non-random diffraction intensity distributions. Those lead to non-random distributions of crystal orientations when analyzed with BEARTEX, although pole figures from EBSD data clearly show random crystal orientations. In an attempt to solve this problem, we employed a scanning routine when recording in-situ synchrotron X-ray diffraction and so collected diffraction from multiple sample volumes rather than from one single spot. Here, we will present a comparison of pole figures derived from independent BEARTEX and EBSD analyses for a series of novaculite experiments and discuss the practicability of BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz. REFERENCES C. BOLLINGER, S. MERKEL AND P. RATERRON (2012): In situ quantitative analysis of stress and texture development in forsterite aggregates deformed at 6 GPa and 1373 K. J. Appl. Cryst., 45, 263-271.

Sucrose lyophiles: a semi-quantitative study of residual water content by total X-ray diffraction analysis.

PubMed

Bates, S; Jonaitis, D; Nail, S

2013-10-01

Total X-ray Powder Diffraction Analysis (TXRPD) using transmission geometry was able to observe significant variance in measured powder patterns for sucrose lyophilizates with differing residual water contents. Integrated diffraction intensity corresponding to the observed variances was found to be linearly correlated to residual water content as measured by an independent technique. The observed variance was concentrated in two distinct regions of the lyophilizate powder pattern, corresponding to the characteristic sucrose matrix double halo and the high angle diffuse region normally associated with free-water. Full pattern fitting of the lyophilizate powder patterns suggested that the high angle variance was better described by the characteristic diffraction profile of a concentrated sucrose/water system rather than by the free-water diffraction profile. This suggests that the residual water in the sucrose lyophilizates is intimately mixed at the molecular level with sucrose molecules forming a liquid/solid solution. The bound nature of the residual water and its impact on the sucrose matrix gives an enhanced diffraction response between 3.0 and 3.5 beyond that expected for free-water. The enhanced diffraction response allows semi-quantitative analysis of residual water contents within the studied sucrose lyophilizates to levels below 1% by weight. Copyright © 2013 Elsevier B.V. All rights reserved.

Crystallization and preliminary X-ray diffraction studies of the glutaminyl cyclase from Carica papaya latex

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

Azarkan, Mohamed; Clantin, Bernard; Bompard, Coralie

2005-01-01

The glutaminyl cyclase isolated from C. papaya latex has been crystallized using the hanging-drop method. Diffraction data have been collected at ESRF beamline BM14 and processed to 1.7 Å resolution. In living systems, the intramolecular cyclization of N-terminal glutamine residues is accomplished by glutaminyl cyclase enzymes (EC 2.3.2.5). While in mammals these enzymes are involved in the synthesis of hormonal and neurotransmitter peptides, the physiological role played by the corresponding plant enzymes still remains to be unravelled. Papaya glutaminyl cyclase (PQC), a 33 kDa enzyme found in the latex of the tropical tree Carica papaya, displays an exceptional resistance tomore » chemical and thermal denaturation as well as to proteolysis. In order to elucidate its enzymatic mechanism and to gain insights into the structural determinants underlying its remarkable stability, PQC was isolated from papaya latex, purified and crystallized by the hanging-drop vapour-diffusion method. The crystals belong to the orthorhombic space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 62.82, b = 81.23, c = 108.17 Å and two molecules per asymmetric unit. Diffraction data have been collected at ESRF beamline BM14 and processed to a resolution of 1.7 Å.« less

Analysis of Short and Long Range Atomic Order in Nanocrystalline Diamonds with Application of Powder Diffractometry

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Neuefiend, J.; Weber, H.-P.; Proffen, T.; VonDreele, R.; Palosz, W.;

Energy research with neutrons (ErwiN) and installation of a fast neutron powder diffraction option at the MLZ, Germany1

PubMed Central

Mühlbauer, Martin J.

2018-01-01

The need for rapid data collection and studies of small sample volumes in the range of cubic millimetres are the main driving forces for the concept of a new high-throughput monochromatic diffraction instrument at the Heinz Maier-Leibnitz Zentrum (MLZ), Germany. A large region of reciprocal space will be accessed by a detector with sufficient dynamic range and microsecond time resolution, while allowing for a variety of complementary sample environments. The medium-resolution neutron powder diffraction option for ‘energy research with neutrons’ (ErwiN) at the high-flux FRM II neutron source at the MLZ is foreseen to meet future demand. ErwiN will address studies of energy-related systems and materials with respect to their structure and uniformity by means of bulk and spatially resolved neutron powder diffraction. A set of experimental options will be implemented, enabling time-resolved studies, rapid parametric measurements as a function of external parameters and studies of small samples using an adapted radial collimator. The proposed powder diffraction option ErwiN will bridge the gap in functionality between the high-resolution powder diffractometer SPODI and the time-of-flight diffractometers POWTEX and SAPHiR at the MLZ. PMID:29896055

National Synchrotron Light Source annual report 1991

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

Hulbert, S.L.; Lazarz, N.M.

1992-04-01

This report discusses the following research conducted at NSLS: atomic and molecular science; energy dispersive diffraction; lithography, microscopy and tomography; nuclear physics; UV photoemission and surface science; x-ray absorption spectroscopy; x-ray scattering and crystallography; x-ray topography; workshop on surface structure; workshop on electronic and chemical phenomena at surfaces; workshop on imaging; UV FEL machine reviews; VUV machine operations; VUV beamline operations; VUV storage ring parameters; x-ray machine operations; x-ray beamline operations; x-ray storage ring parameters; superconducting x-ray lithography source; SXLS storage ring parameters; the accelerator test facility; proposed UV-FEL user facility at the NSLS; global orbit feedback systems; and NSLSmore » computer system.« less

Low-aberration beamline optics for synchrotron infrared nanospectroscopy.

PubMed

Freitas, Raul O; Deneke, Christoph; Maia, Francisco C B; Medeiros, Helton G; Moreno, Thierry; Dumas, Paul; Petroff, Yves; Westfahl, Harry

2018-04-30

Synchrotron infrared nanospectroscopy is a recently developed technique that enables new possibilities in the broadband chemical analysis of materials in the nanoscale, far beyond the diffraction limit in this frequency domain. Synchrotron infrared ports have exploited mainly the high brightness advantage provided by electron storage rings across the whole infrared range. However, optical aberrations in the beam produced by the source depth of bending magnet emission at large angles prevent infrared nanospectroscopy to reach its maximum capability. In this work we present a low-aberration optical layout specially designed and constructed for a dedicated synchrotron infrared nanospectroscopy beamline. We report excellent agreement between simulated beam profiles (from standard wave propagation and raytracing optics simulations) with experimental measurements. We report an important improvement in the infrared nanospectroscopy experiment related to the improved beamline optics. Finally, we demonstrate the performance of the nanospectroscopy endstation by measuring a hyperspectral image of a polar material and we evaluate the setup sensitivity by measuring ultra-thin polymer films down to 6 nm thick.

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

PubMed

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

2004-05-01

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

Projection x-ray topography system at 1-BM x-ray optics test beamline at the advanced photon source

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

Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Liu, Zunping; Trakhtenberg, Emil

2016-07-27

Projection X-ray topography of single crystals is a classic technique for the evaluation of intrinsic crystal quality of large crystals. In this technique a crystal sample and an area detector (e.g., X-ray film) collecting intensity of a chosen crystallographic reflection are translated simultaneously across an X-ray beam collimated in the diffraction scattering plane (e.g., [1, 2]). A bending magnet beamline of a third-generation synchrotron source delivering x-ray beam with a large horizontal divergence, and therefore, a large horizontal beam size at a crystal sample position offers an opportunity to obtain X-ray topographs of large crystalline samples (e.g., 6-inch wafers) inmore » just a few exposures. Here we report projection X-ray topography system implemented recently at 1-BM beamline of the Advanced Photon Source. A selected X-ray topograph of a 6-inch wafer of 4H-SiC illustrates capabilities and limitations of the technique.« less

Synthesis and luminescent properties of Gd3Ga2Al3O12 phosphors doped with Eu3+ or Ce3+

NASA Astrophysics Data System (ADS)

Oh, M. J.; Kim, H. J.

2016-09-01

Eu3+-or Ce3+-doped gadolinium gallium aluminum garnet (GGAG), Gd3Ga2Al3O12, phosphors are fabricated using solid-state reactions with Gd2O3, Ga2O3, Al2O3, CeO2 and Eu2O3 powders. The Eu3+-or Ce3+-doped Gd3Ga2Al3O12 phosphors are sintered at 1300 °C or 1600 °C for 5 hours by using an electric furnace under normal atmosphere. X-ray diffraction and field-emission scanning electron microscopy studies are carried out in order to analyze the physical properties of these materials, and their luminescence properties are also measured by using UV and X-ray sources. The Eu3+-or Ce3+-doped Gd3Ga2Al3O12 phosphors show higher light yields in comparison to commercial phosphors such as Gd2O2S:Tb (gadox). This indicates that Gd3Ga2Al3O12:Eu3+ phosphors are promising materials for use in X-ray imaging and dose monitoring at proton beamlines.

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

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

Balagurov, Anatoly M.; Bobrikov, Ivan A.; Bokuchava, Gizo D.

2015-11-15

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of themore » material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.« less

Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

PubMed Central

Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

2018-01-01

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

Structure determination of Ba5AlF13 by coupling electron, synchrotron and neutron powder diffraction, solid-state NMR and ab initio calculations.

PubMed

Martineau, Charlotte; Allix, Mathieu; Suchomel, Matthew R; Porcher, Florence; Vivet, François; Legein, Christophe; Body, Monique; Massiot, Dominique; Taulelle, Francis; Fayon, Franck

2016-10-04

The room temperature structure of Ba 5 AlF 13 has been investigated by coupling electron, synchrotron and neutron powder diffraction, solid-state high-resolution NMR ( 19 F and 27 Al) and first principles calculations. An initial structural model has been obtained from electron and synchrotron powder diffraction data, and its main features have been confirmed by one- and two-dimensional NMR measurements. However, DFT GIPAW calculations of the 19 F isotropic shieldings revealed an inaccurate location of one fluorine site (F3, site 8a), which exhibited unusual long F-Ba distances. The atomic arrangement was reinvestigated using neutron powder diffraction data. Subsequent Fourier maps showed that this fluorine atom occupies a crystallographic site of lower symmetry (32e) with partial occupancy (25%). GIPAW computations of the NMR parameters validate the refined structural model, ruling out the presence of local static disorder and indicating that the partial occupancy of this F site reflects a local motional process. Visualisation of the dynamic process was then obtained from the Rietveld refinement of neutron diffraction data using an anharmonic description of the displacement parameters to account for the thermal motion of the mobile fluorine. The whole ensemble of powder diffraction and NMR data, coupled with first principles calculations, allowed drawing an accurate structural model of Ba 5 AlF 13 , including site-specific dynamical disorder in the fluorine sub-network.

A new theory for X-ray diffraction.

PubMed

Fewster, Paul F

2014-05-01

This article proposes a new theory of X-ray scattering that has particular relevance to powder diffraction. The underlying concept of this theory is that the scattering from a crystal or crystallite is distributed throughout space: this leads to the effect that enhanced scatter can be observed at the `Bragg position' even if the `Bragg condition' is not satisfied. The scatter from a single crystal or crystallite, in any fixed orientation, has the fascinating property of contributing simultaneously to many `Bragg positions'. It also explains why diffraction peaks are obtained from samples with very few crystallites, which cannot be explained with the conventional theory. The intensity ratios for an Si powder sample are predicted with greater accuracy and the temperature factors are more realistic. Another consequence is that this new theory predicts a reliability in the intensity measurements which agrees much more closely with experimental observations compared to conventional theory that is based on `Bragg-type' scatter. The role of dynamical effects (extinction etc.) is discussed and how they are suppressed with diffuse scattering. An alternative explanation for the Lorentz factor is presented that is more general and based on the capture volume in diffraction space. This theory, when applied to the scattering from powders, will evaluate the full scattering profile, including peak widths and the `background'. The theory should provide an increased understanding of the reliability of powder diffraction measurements, and may also have wider implications for the analysis of powder diffraction data, by increasing the accuracy of intensities predicted from structural models.

I12: the Joint Engineering, Environment and Processing (JEEP) beamline at Diamond Light Source.

PubMed

Drakopoulos, Michael; Connolley, Thomas; Reinhard, Christina; Atwood, Robert; Magdysyuk, Oxana; Vo, Nghia; Hart, Michael; Connor, Leigh; Humphreys, Bob; Howell, George; Davies, Steve; Hill, Tim; Wilkin, Guy; Pedersen, Ulrik; Foster, Andrew; De Maio, Nicoletta; Basham, Mark; Yuan, Fajin; Wanelik, Kaz

2015-05-01

I12 is the Joint Engineering, Environmental and Processing (JEEP) beamline, constructed during Phase II of the Diamond Light Source. I12 is located on a short (5 m) straight section of the Diamond storage ring and uses a 4.2 T superconducting wiggler to provide polychromatic and monochromatic X-rays in the energy range 50-150 keV. The beam energy enables good penetration through large or dense samples, combined with a large beam size (1 mrad horizontally × 0.3 mrad vertically). The beam characteristics permit the study of materials and processes inside environmental chambers without unacceptable attenuation of the beam and without the need to use sample sizes which are atypically small for the process under study. X-ray techniques available to users are radiography, tomography, energy-dispersive diffraction, monochromatic and white-beam two-dimensional diffraction/scattering and small-angle X-ray scattering. Since commencing operations in November 2009, I12 has established a broad user community in materials science and processing, chemical processing, biomedical engineering, civil engineering, environmental science, palaeontology and physics.

Automatic sample Dewar for MX beam-line

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

Charignon, T.; Tanchon, J.; Trollier, T.

2014-01-29

It is very common for crystals of large biological macromolecules to show considerable variation in quality of their diffraction. In order to increase the number of samples that are tested for diffraction quality before any full data collections at the ESRF*, an automatic sample Dewar has been implemented. Conception and performances of the Dewar are reported in this paper. The automatic sample Dewar has 240 samples capability with automatic loading/unloading ports. The storing Dewar is capable to work with robots and it can be integrated in a full automatic MX** beam-line. The samples are positioned in the front of themore » loading/unloading ports with and automatic rotating plate. A view port has been implemented for data matrix camera reading on each sample loaded in the Dewar. At last, the Dewar is insulated with polyurethane foam that keeps the liquid nitrogen consumption below 1.6 L/h. At last, the static insulation also makes vacuum equipment and maintenance unnecessary. This Dewar will be useful for increasing the number of samples tested in synchrotrons.« less

Optical and x-ray alignment approaches for off-plane reflection gratings

NASA Astrophysics Data System (ADS)

Allured, Ryan; Donovan, Benjamin D.; DeRoo, Casey T.; Marlowe, Hannah R.; McEntaffer, Randall L.; Tutt, James H.; Cheimets, Peter N.; Hertz, Edward; Smith, Randall K.; Burwitz, Vadim; Hartner, Gisela; Menz, Benedikt

2015-09-01

Off-plane reflection gratings offer the potential for high-resolution, high-throughput X-ray spectroscopy on future missions. Typically, the gratings are placed in the path of a converging beam from an X-ray telescope. In the off-plane reflection grating case, these gratings must be co-aligned such that their diffracted spectra overlap at the focal plane. Misalignments degrade spectral resolution and effective area. In-situ X-ray alignment of a pair of off-plane reflection gratings in the path of a silicon pore optics module has been performed at the MPE PANTER beamline in Germany. However, in-situ X-ray alignment may not be feasible when assembling all of the gratings required for a satellite mission. In that event, optical methods must be developed to achieve spectral alignment. We have developed an alignment approach utilizing a Shack-Hartmann wavefront sensor and diffraction of an ultraviolet laser. We are fabricating the necessary hardware, and will be taking a prototype grating module to an X-ray beamline for performance testing following assembly and alignment.

I12: the Joint Engineering, Environment and Processing (JEEP) beamline at Diamond Light Source

PubMed Central

Drakopoulos, Michael; Connolley, Thomas; Reinhard, Christina; Atwood, Robert; Magdysyuk, Oxana; Vo, Nghia; Hart, Michael; Connor, Leigh; Humphreys, Bob; Howell, George; Davies, Steve; Hill, Tim; Wilkin, Guy; Pedersen, Ulrik; Foster, Andrew; De Maio, Nicoletta; Basham, Mark; Yuan, Fajin; Wanelik, Kaz

2015-01-01

I12 is the Joint Engineering, Environmental and Processing (JEEP) beamline, constructed during Phase II of the Diamond Light Source. I12 is located on a short (5 m) straight section of the Diamond storage ring and uses a 4.2 T superconducting wiggler to provide polychromatic and monochromatic X-rays in the energy range 50–150 keV. The beam energy enables good penetration through large or dense samples, combined with a large beam size (1 mrad horizontally × 0.3 mrad vertically). The beam characteristics permit the study of materials and processes inside environmental chambers without unacceptable attenuation of the beam and without the need to use sample sizes which are atypically small for the process under study. X-ray techniques available to users are radiography, tomography, energy-dispersive diffraction, monochromatic and white-beam two-dimensional diffraction/scattering and small-angle X-ray scattering. Since commencing operations in November 2009, I12 has established a broad user community in materials science and processing, chemical processing, biomedical engineering, civil engineering, environmental science, palaeontology and physics. PMID:25931103

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl(6) and other alloys are twinned cubic crystals.

PubMed

Pauling, L

1987-06-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl(6) and Mg(32)(Al,Zn)(49) and the neutron powder diffraction pattern of MnAl(6) are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 A (x-ray) and 23.416 A (neutron) for MnAl(6) and 24.313 A (x-ray) for Mg(32)(Al,Zn)(49).

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl6 and other alloys are twinned cubic crystals

PubMed Central

Pauling, Linus

1987-01-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl6 and Mg32(Al,Zn)49 and the neutron powder diffraction pattern of MnAl6 are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 Å (x-ray) and 23.416 Å (neutron) for MnAl6 and 24.313 Å (x-ray) for Mg32(Al,Zn)49. PMID:16593841

New high- and low-temperature apparatus for synchrotron polycrystalline X-ray diffraction.

PubMed

Tang, C C; Bushnell-Wye, G; Cernik, R J

1998-05-01

A high-temperature furnace with an induction heater coil and a cryogenic system based on closed-cycle refrigeration have been assembled to enhance the non-ambient powder diffraction facilities at the Synchrotron Radiation Source, Daresbury Laboratory. The commissioning of the high- and low-temperature devices on the high-resolution powder diffractometer of Station 2.3 is described. The combined temperature range provided by the furnace/cryostat is 10-1500 K. Results from Fe and NH(4)Br powder samples are presented to demonstrate the operation of the apparatus. The developments presented in this paper are applicable to a wide range of other experiments and diffraction geometries.

Scanning three-dimensional x-ray diffraction microscopy using a high-energy microbeam

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

Hayashi, Y., E-mail: y-hayashi@mosk.tytlabs.co.jp; Hirose, Y.; Seno, Y.

2016-07-27

A scanning three-dimensional X-ray diffraction (3DXRD) microscope apparatus with a high-energy microbeam was installed at the BL33XU Toyota beamline at SPring-8. The size of the 50 keV beam focused using Kirkpatrick-Baez mirrors was 1.3 μm wide and 1.6 μm high in full width at half maximum. The scanning 3DXRD method was tested for a cold-rolled carbon steel sheet sample. A three-dimensional orientation map with 37 {sup 3} voxels was obtained.

Diffraction properties of multilayer Laue lenses with an aperture of 102 µm and WSi 2/Al bilayers

DOE PAGES

Kubec, Adam; Kujala, Naresh; Conley, Raymond; ...

2015-01-01

Here, we report on the characterization of a multilayer Laue lens (MLL) with large acceptance, made of a novel WSi2/Al bilayer system. Fabrication of multilayers with large deposition thickness is required to obtain MLL structures with sufficient apertures capable of accepting the full lateral coherence length of x-rays at typical nanofocusing beamlines. To date, the total deposition thickness has been limited by stress-buildup in the multilayer. We were able to grow WSi2/Al with low grown-in stress, and asses the degree of stress reduction. X-ray diffraction experiments were conducted at beamline 1-BM at the Advanced Photon Source. We used monochromatic x-raysmore » with a photon energy of 12 keV and a bandwidth of ΔE/E=5.4 ∙ 10 -4. The MLL was grown with parallel layer interfaces, and was designed to have a large focal length of 9.6 mm. The mounted lens was 2.7 mm in width. We found and quantified kinks and bending of sections of the MLL. Sections with bending were found to partly have a systematic progression in the interface angles. We also observed kinking in some, but not all, areas. The measurements are compared with dynamic diffraction calculations made with Coupled Wave Theory. Finally our data are plotted showing the diffraction efficiency as a function of the external tilting angle of the entire mounted lens. This way of plotting the data was found to provide an overview into the diffraction properties of the whole lens, and enabled the following layer tilt analyses.« less

Improved camera for better X-ray powder photographs

NASA Technical Reports Server (NTRS)

Parrish, W.; Vajda, I. E.

1969-01-01

Camera obtains powder-type photographs of single crystals or polycrystalline powder specimens. X-ray diffraction photographs of a powder specimen are characterized by improved resolution and greater intensity. A reasonably good powder pattern of small samples can be produced for identification purposes.

APS 6BM-B Large Volume High Pressure Beamline: A Workhorse for Rock and Mineral Physics

NASA Astrophysics Data System (ADS)

Chen, H.; Whitaker, M. L.; Baldwin, K. J.; Huebsch, W. R.; Vaughan, M. T.; Weidner, D. J.

2017-12-01

With the inheritance of decades of technical innovations at the NSLS X17B2 Beamline, APS 6BM-B Beamline was established in 2015 and is a dedicated beamline for synchrotron-based large volume high pressure research in earth sciences, especially rock and mineral physics. Currently a 250-ton hydraulic press equipped with a D-DIA module is installed and a Rotational Drickamer Apparatus from Yale University is hosted every cycle, covering a pressure range from crust to lower mantle. 6BM-B operates in white beam mode with an effective energy range of 20-100 keV. Energy dispersive X-ray diffraction data is collected using a 10-element solid state Ge array detector arranged in a circular geometry to allow for the real time assessment of stress. Direct radiographic imaging using Prosillica CCD camera and scintillating YAG crystals yields sample strain and strain rate. In addition to applications in phase transitions, equation of states measurements, sound velocity measurements, this setup is ideal for studies of steady state and dynamic deformation process. In this presentation, technical features and strengths of 6BM-B will be discussed. Most recent progress and science highlights of our user community will be showcased.

EPICS controlled sample mounting robots at the GM/CA CAT.

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

Makarov, O. A.; Benn, R.; Corcoran, S.

2007-11-11

GM/CA CAT at Sector 23 of the advanced photon source (APS) is an NIH funded facility for crystallographic structure determination of biological macromolecules by X-ray diffraction [R.F. Fischetti, et al., GM/CA canted undulator beamlines for protein crystallography, Acta Crystallogr. A 61 (2005) C139]. The facility consists of three beamlines; two based on canted undulators and one on a bending magnet. The scientific and technical goals of the CAT emphasize streamlined, efficient throughput for a variety of sample types, sizes and qualities, representing the cutting edge of structural biology research. For this purpose all three beamlines are equipped with the ALS-stylemore » robots [C.W.Cork, et al. Status of the BCSB automated sample mounting and alignment system for macromolecular crystallography at the Advanced Light Source, SRI-2003, San-Francisco, CA, USA, August 25-29, 2003] for an automated mounting of cryo-protected macromolecular crystals. This report summarizes software and technical solutions implemented with the first of the three operational robots at beamline 23-ID-B. The automounter's Dewar can hold up to 72 or 96 samples residing in six Rigaku ACTOR magazines or ALS-style pucks, respectively. Mounting of a crystal takes approximately 2 s, during which time the temperature of the crystal is maintained near that of liquid nitrogen.« less

Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

NASA Astrophysics Data System (ADS)

Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

2015-10-01

The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

A new theory for X-ray diffraction

PubMed Central

Fewster, Paul F.

2014-01-01

This article proposes a new theory of X-ray scattering that has particular relevance to powder diffraction. The underlying concept of this theory is that the scattering from a crystal or crystallite is distributed throughout space: this leads to the effect that enhanced scatter can be observed at the ‘Bragg position’ even if the ‘Bragg condition’ is not satisfied. The scatter from a single crystal or crystallite, in any fixed orientation, has the fascinating property of contributing simultaneously to many ‘Bragg positions’. It also explains why diffraction peaks are obtained from samples with very few crystallites, which cannot be explained with the conventional theory. The intensity ratios for an Si powder sample are predicted with greater accuracy and the temperature factors are more realistic. Another consequence is that this new theory predicts a reliability in the intensity measurements which agrees much more closely with experimental observations compared to conventional theory that is based on ‘Bragg-type’ scatter. The role of dynamical effects (extinction etc.) is discussed and how they are suppressed with diffuse scattering. An alternative explanation for the Lorentz factor is presented that is more general and based on the capture volume in diffraction space. This theory, when applied to the scattering from powders, will evaluate the full scattering profile, including peak widths and the ‘background’. The theory should provide an increased understanding of the reliability of powder diffraction measurements, and may also have wider implications for the analysis of powder diffraction data, by increasing the accuracy of intensities predicted from structural models. PMID:24815975

National Synchrotron Light Source annual report 1991. Volume 1, October 1, 1990--September 30, 1991

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

Hulbert, S.L.; Lazarz, N.M.

1992-04-01

This report discusses the following research conducted at NSLS: atomic and molecular science; energy dispersive diffraction; lithography, microscopy and tomography; nuclear physics; UV photoemission and surface science; x-ray absorption spectroscopy; x-ray scattering and crystallography; x-ray topography; workshop on surface structure; workshop on electronic and chemical phenomena at surfaces; workshop on imaging; UV FEL machine reviews; VUV machine operations; VUV beamline operations; VUV storage ring parameters; x-ray machine operations; x-ray beamline operations; x-ray storage ring parameters; superconducting x-ray lithography source; SXLS storage ring parameters; the accelerator test facility; proposed UV-FEL user facility at the NSLS; global orbit feedback systems; and NSLSmore » computer system.« less

Atomic pair distribution function at the Brazilian Synchrotron Light Laboratory: application to the Pb 1–x La xZr 0.40Ti 0.60O 3 ferroelectric system

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

Saleta, M. E.; Eleotério, M.; Mesquita, A.

2017-07-29

This work reports the setting up of the X-ray diffraction and spectroscopy beamline at the Brazilian Synchrotron Light Laboratory for performing total scattering experiments to be analyzed by atomic pair distribution function (PDF) studies. The results of a PDF refinement for Al 2O 3 standard are presented and compared with data acquired at a beamline of the Advanced Photon Source, where it is common to perform this type of experiment. A preliminary characterization of the Pb 1–xLa xZr 0.40Ti 0.60O 3 ferroelectric system, withx= 0.11, 0.12 and 0.15, is also shown.

Control system for the 2nd generation Berkeley AutoMounters (BAM2) at GM/CA CAT macromolecular crystallography beamlines

PubMed Central

Makarov, O.; Hilgart, M.; Ogata, C.; Pothineni, S.; Cork, C.

2011-01-01

GM/CA CAT at Sector 23 of the Advanced Photon Source (APS) is an NIH funded facility for crystallographic structure determination of biological macromolecules by X-ray diffraction. A second generation Berkeley automounter is being integrated into the beamline control system at the 23-BM experimental station. This new device replaces the previous all-pneumatic gripper motions with a combination of pneumatics and XYZ motorized linear stages. The latter adds a higher degree of flexibility to the robot including auto-alignment capability, accommodation of a larger capacity sample Dewar of arbitrary shape, and support for advanced operations such as crystal washing, while preserving the overall simplicity and efficiency of the Berkeley automounter design. PMID:21822343

HiSPoD: a program for high-speed polychromatic X-ray diffraction experiments and data analysis on polycrystalline samples

DOE PAGES

Sun, Tao; Fezzaa, Kamel

2016-06-17

Here, a high-speed X-ray diffraction technique was recently developed at the 32-ID-B beamline of the Advanced Photon Source for studying highly dynamic, yet non-repeatable and irreversible, materials processes. In experiments, the microstructure evolution in a single material event is probed by recording a series of diffraction patterns with extremely short exposure time and high frame rate. Owing to the limited flux in a short pulse and the polychromatic nature of the incident X-rays, analysis of the diffraction data is challenging. Here, HiSPoD, a stand-alone Matlab-based software for analyzing the polychromatic X-ray diffraction data from polycrystalline samples, is described. With HiSPoD,more » researchers are able to perform diffraction peak indexing, extraction of one-dimensional intensity profiles by integrating a two-dimensional diffraction pattern, and, more importantly, quantitative numerical simulations to obtain precise sample structure information.« less

A new high temperature reactor for operando XAS: Application for the dry reforming of methane over Ni/ZrO2 catalyst.

PubMed

Aguilar-Tapia, Antonio; Ould-Chikh, Samy; Lahera, Eric; Prat, Alain; Delnet, William; Proux, Olivier; Kieffer, Isabelle; Basset, Jean-Marie; Takanabe, Kazuhiro; Hazemann, Jean-Louis

2018-03-01

The construction of a high-temperature reaction cell for operando X-ray absorption spectroscopy characterization is reported. A dedicated cell was designed to operate as a plug-flow reactor using powder samples requiring gas flow and thermal treatment at high temperatures. The cell was successfully used in the reaction of dry reforming of methane (DRM). We present X-ray absorption results in the fluorescence detection mode on a 0.4 wt. % Ni/ZrO 2 catalyst under realistic conditions at 750 °C, reproducing the conditions used for a conventional dynamic microreactor for the DRM reaction. The setup includes a gas distribution system that can be fully remotely operated. The reaction cell offers the possibility of transmission and fluorescence detection modes. The complete setup dedicated to the study of catalysts is permanently installed on the Collaborating Research Groups French Absorption spectroscopy beamline in Material and Environmental sciences (CRG-FAME) and French Absorption spectroscopy beamline in Material and Environmental sciences at Ultra-High Dilution (FAME-UHD) beamlines (BM30B and BM16) at the European Synchrotron Radiation Facility in Grenoble, France.

A new high temperature reactor for operando XAS: Application for the dry reforming of methane over Ni/ZrO2 catalyst

NASA Astrophysics Data System (ADS)

Aguilar-Tapia, Antonio; Ould-Chikh, Samy; Lahera, Eric; Prat, Alain; Delnet, William; Proux, Olivier; Kieffer, Isabelle; Basset, Jean-Marie; Takanabe, Kazuhiro; Hazemann, Jean-Louis

2018-03-01

The construction of a high-temperature reaction cell for operando X-ray absorption spectroscopy characterization is reported. A dedicated cell was designed to operate as a plug-flow reactor using powder samples requiring gas flow and thermal treatment at high temperatures. The cell was successfully used in the reaction of dry reforming of methane (DRM). We present X-ray absorption results in the fluorescence detection mode on a 0.4 wt. % Ni/ZrO2 catalyst under realistic conditions at 750 °C, reproducing the conditions used for a conventional dynamic microreactor for the DRM reaction. The setup includes a gas distribution system that can be fully remotely operated. The reaction cell offers the possibility of transmission and fluorescence detection modes. The complete setup dedicated to the study of catalysts is permanently installed on the Collaborating Research Groups French Absorption spectroscopy beamline in Material and Environmental sciences (CRG-FAME) and French Absorption spectroscopy beamline in Material and Environmental sciences at Ultra-High Dilution (FAME-UHD) beamlines (BM30B and BM16) at the European Synchrotron Radiation Facility in Grenoble, France.

Equation of State of Iron-Rich (Mg,Fe)O

NASA Astrophysics Data System (ADS)

Dobrosavljevic, V.; Jackson, J. M.

2017-12-01

Recent seismic observations of the core-mantle boundary (CMB) have provided increasing evidence for the presence of a boundary layer rich in chemical diversity with lateral variations in seismic velocities and densities. Exploring causes of observed anomalies such as ultralow-velocity zones (ULVZs) in this region can lead to a deeper understanding of phenomena like hotspot volcanism and heat flow from the core. One potential explanation for the presence of these lateral heterogeneities may be iron enrichment in lower mantle minerals such as magnesiowüstite, possibly resulting from melting events or interactions with the iron-dominant outer core. Relatively little study has been directed toward iron-rich members of the (Mg,Fe)O solid solution despite the possibility for even low levels of iron enrichment to have significant impact on elastic properties. To that end, we present results from a powder x-ray diffraction study on (Mg0.06Fe0.94)O up to 90 GPa at 300 K using helium as a pressure-transmitting medium. The measurements were conducted at beamline 12.2.2 of the Advanced Light Source of Lawrence Berkeley National Laboratory. The diffraction data were used to determine the equations of state for the material's B1 cubic and rhombohedral phases and constrain the transition pressure at ambient temperature. We combine our results with pressure-temperature-volume measurements on an identical composition (Wicks et al. 2015) to produce a well-constrained thermal equation of state. Using these results, we report a thermal elasticity model for magnesiowüstite at CMB conditions for use in dynamic modeling and comparison against seismic observations.

Synchrotron X-ray powder diffraction data of LASSBio-1515: A new N-acylhydrazone derivative compound

NASA Astrophysics Data System (ADS)

Costa, F. N.; Braz, D.; Ferreira, F. F.; da Silva, T. F.; Barreiro, E. J.; Lima, L. M.; Colaço, M. V.; Kuplich, L.; Barroso, R. C.

2014-02-01

In this work, synchrotron X-ray powder diffraction data allowed for a successful indexing of LASSBio-1515 compound, candidate to analgesic and anti-inflammatory activity. X-ray powder diffraction data collected in transmission and high-throughput geometries were used to analyze this compound. The X-ray wavelength of the synchrotron radiation used in this study was determined to be λ=1.55054 Å. LASSBio-1515 was found to be monoclinic with space group P21/c and unit cell parameters a=11.26255(16) Å, b=12.59785(16) Å, c=8.8540(1) Å, β=90.5972(7)° and V=1256.17(3) Å3.

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

DOE PAGES

Fan, D.; Huang, J. W.; Zeng, X. L.; ...

2016-05-23

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.« less

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

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

Fan, D.; Huang, J. W.; Zeng, X. L.

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.« less

Observations on online educational materials for powder diffraction crystallography software.

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

Toby, B. H.

2010-10-01

This article presents a series of approaches used to educate potential users of crystallographic software for powder diffraction. The approach that has been most successful in the author's opinion is the web lecture, where an audio presentation is coupled to a video-like record of the contents of the presenter's computer screen.

Swinging Symmetry, Multiple Structural Phase Transitions, and Versatile Physical Properties in RECuGa3 (RE = La-Nd, Sm-Gd).

PubMed

Subbarao, Udumula; Rayaprol, Sudhindra; Dally, Rebecca; Graf, Michael J; Peter, Sebastian C

2016-01-19

The compounds RECuGa3 (RE = La-Nd, Sm-Gd) were synthesized by various techniques. Preliminary X-ray diffraction (XRD) analyses at room temperature suggested that the compounds crystallize in the tetragonal system with either the centrosymmetric space group I4/mmm (BaAl4 type) or the non-centrosymmetric space group I4mm (BaNiSn3 type). Detailed single-crystal XRD, neutron diffraction, and synchrotron XRD studies of selected compounds confirmed the non-centrosymmetric BaNiSn3 structure type at room temperature with space group I4mm. Temperature-dependent single-crystal XRD, powder XRD, and synchrotron beamline measurements showed a structural transition between centro- and non-centrosymmetry followed by a phase transition to the Rb5Hg19 type (space group I4/m) above 400 K and another transition to the Cu3Au structure type (space group Pm3̅m) above 700 K. Combined single-crystal and synchrotron powder XRD studies of PrCuGa3 at high temperatures revealed structural transitions at higher temperatures, highlighting the closeness of the BaNiSn3 structure to other structure types not known to the RECuGa3 family. The crystal structure of RECuGa3 is composed of eight capped hexagonal prism cages [RE4Cu4Ga12] occupying one rare-earth atom in each ring, which are shared through the edge of Cu and Ga atoms along the ab plane, resulting in a three-dimensional network. Resistivity and magnetization measurements demonstrated that all of these compounds undergo magnetic ordering at temperatures between 1.8 and 80 K, apart from the Pr and La compounds: the former remains paramagnetic down to 0.3 K, while superconductivity was observed in the La compound at T = 1 K. It is not clear whether this is intrinsic or due to filamentary Ga present in the sample. The divalent nature of Eu in EuCuGa3 was confirmed by magnetization measurements and X-ray absorption near edge spectroscopy and is further supported by the crystal structure analysis.

Frequency analysis for modulation-enhanced powder diffraction.

PubMed

Chernyshov, Dmitry; Dyadkin, Vadim; van Beek, Wouter; Urakawa, Atsushi

2016-07-01

Periodic modulation of external conditions on a crystalline sample with a consequent analysis of periodic diffraction response has been recently proposed as a tool to enhance experimental sensitivity for minor structural changes. Here the intensity distributions for both a linear and nonlinear structural response induced by a symmetric and periodic stimulus are analysed. The analysis is further extended for powder diffraction when an external perturbation changes not only the intensity of Bragg lines but also their positions. The derived results should serve as a basis for a quantitative modelling of modulation-enhanced diffraction data measured in real conditions.

SPring-8 BL41XU, a high-flux macromolecular crystallography beamline

PubMed Central

Hasegawa, Kazuya; Shimizu, Nobutaka; Okumura, Hideo; Mizuno, Nobuhiro; Baba, Seiki; Hirata, Kunio; Takeuchi, Tomoyuki; Yamazaki, Hiroshi; Senba, Yasunori; Ohashi, Haruhiko; Yamamoto, Masaki; Kumasaka, Takashi

2013-01-01

SPring-8 BL41XU is a high-flux macromolecular crystallography beamline using an in-vacuum undulator as a light source. The X-rays are monochromated by a liquid-nitrogen-cooling Si double-crystal monochromator, and focused by Kirkpatrick–Baez mirror optics. The focused beam size at the sample is 80 µm (H) × 22 µm (V) with a photon flux of 1.1 × 1013 photons s−1. A pinhole aperture is used to collimate the beam in the range 10–50 µm. This high-flux beam with variable size provides opportunities not only for micro-crystallography but also for data collection effectively making use of crystal volume. The beamline also provides high-energy X-rays covering 20.6–35.4 keV which allows ultra-high-resolution data to be obtained and anomalous diffraction using the K-edge of Xe and I. Upgrade of BL41XU for more rapid and accurate data collection is proceeding. Here, details of BL41XU are given and an outline of the upgrade project is documented. PMID:24121338

Physicochemical characterization and aerosol dispersion performance of organic solution advanced spray-dried cyclosporine A multifunctional particles for dry powder inhalation aerosol delivery

PubMed Central

Wu, Xiao; Zhang, Weifen; Hayes, Don; Mansour, Heidi M

2013-01-01

In this systematic and comprehensive study, inhalation powders of the polypeptide immunosuppressant drug – cyclosporine A – for lung delivery as dry powder inhalers (DPIs) were successfully designed, developed, and optimized. Several spray drying pump rates were rationally chosen. Comprehensive physicochemical characterization and imaging was carried out using scanning electron microscopy, hot-stage microscopy, differential scanning calorimetry, powder X-ray diffraction, Karl Fischer titration, laser size diffraction, and gravimetric vapor sorption. Aerosol dispersion performance was conducted using a next generation impactor with a Food and Drug Administration-approved DPI device. These DPIs displayed excellent aerosol dispersion performance with high values in emitted dose, respirable fraction, and fine particle fraction. In addition, novel multifunctional inhalation aerosol powder formulations of cyclosporine A with lung surfactant-mimic phospholipids were also successfully designed and developed by advanced organic solution cospray drying in closed mode. The lung surfactantmimic phospholipids were 1,2-dipalmitoyl-sn-glycero-3-phosphocholine and 1,2-dipalmitoyl-snglycero- 3-(phosphor-rac-1-glycerol). These cyclosporine A lung surfactant-mimic aerosol powder formulations were comprehensively characterized. Powder X-ray diffraction and differential scanning calorimetry confirmed that the phospholipid bilayer structure in the solid state was preserved following advanced organic solution spray drying in closed mode. These novel multifunctional inhalation powders were optimized for DPI delivery with excellent aerosol dispersion performance and high aerosol performance parameters. PMID:23569375

The High Resolution Powder Diffraction Beam Line at ESRF.

PubMed

Fitch, A N

2004-01-01

The optical design and performance of the high-resolution powder diffraction beam line BM16 at ESRF are discussed and illustrated. Some recent studies carried out on BM16 are described, including crystal structure solution and refinement, anomalous scattering, in situ measurements, residual strain in engineering components, investigation of microstructure, and grazing-incidence diffraction from surface layers. The beam line is built on a bending magnet, and operates in the energy range from 5 keV to 40 keV. After the move to an undulator source in 2002, it will benefit from an extented energy range up to 60 keV and increased flux and resolution. It is anticipated that enhancements to the data quality will be achieved, leading to the solution of larger crystal structures, and improvements in the accuracy of refined structures. The systematic exploitation of anisotropic thermal expansion will help reduce the effects of peak overlap in the analysis of powder diffraction data.

Application of powder X-ray diffraction in studying the compaction behavior of bulk pharmaceutical powders.

PubMed

Bandyopadhyay, Rebanta; Selbo, Jon; Amidon, Gregory E; Hawley, Michael

2005-11-01

This study investigates the effects of crystal lattice deformation on the powder X-ray diffraction (PXRD) patterns of compressed polycrystalline specimen (compacts/tablets) made from molecular, crystalline powders. The displacement of molecules and the corresponding adjustment of interplanar distances (d-spacings) between diffracting planes of PNU-288034 and PNU-177553, which have crystal habits with a high aspect ratio favoring preferred orientation during tableting, are demonstrated by shifts in the diffracted peak positions. The direction of shift in diffracted peak positions suggests a reduction of interplanar d-spacing in the crystals of PNU-288034 and PNU-177553 following compaction. There is also a general reduction of peak intensities following compression at the different compressive loads. The lattice strain representing the reduction in d-spacing is proportional to the original d-spacing of the uncompressed sample suggesting that, as with systems that obey a simple Hooke's law relationship, the further apart the planes of atoms/molecules within the lattice are, the easier it is for them to approach each other under compressive stresses. For a third model compound comprising more equant-shaped crystals of PNU-141659, the shift in diffracted peak positions are consistent with an expansion of lattice spacing after compression. This apparent anomaly is supported by the PXRD studies of the bulk powder consisting of fractured crystals where also, the shift in peak position suggests expansion of the lattice planes. Thus the crystals of PNU-141659 may be fracturing under the compressive loads used to produce the compacts. Additional studies are underway to relate the PXRD observations with the bulk tableting properties of these model compounds.

Diffractive-refractive optics: X-ray splitter.

PubMed

Hrdý, Jaromír

2010-01-01

The possibility of splitting a thin (e.g. undulator) X-ray beam based on diffraction-refraction effects is discussed. The beam is diffracted from a crystal whose diffracting surface has the shape of a roof with the ridge lying in the plane of diffraction. The crystal is cut asymmetrically. One half of the beam impinges on the left-hand part of the roof and the other half impinges on the right-hand side of the roof. Owing to refraction the left part of the beam is deviated to the left whereas the right part is deviated to the right. The device proposed consists of two channel-cut crystals with roof-like diffraction surfaces; the crystals are set in a dispersive position. The separation of the beams after splitting is calculated at a distance of 10 m from the crystals for various asymmetry and inclination angles. It is shown that such a splitting may be utilized for long beamlines. Advantages and disadvantages of this method are discussed.

A history of neutrons in biology: the development of neutron protein crystallography at BNL and LANL.

PubMed

Schoenborn, Benno P

2010-11-01

The first neutron diffraction data were collected from crystals of myoglobin almost 42 years ago using a step-scan diffractometer with a single detector. Since then, major advances have been made in neutron sources, instrumentation and data collection and analysis, and in biochemistry. Fundamental discoveries about enzyme mechanisms, biological complex structures, protein hydration and H-atom positions have been and continue to be made using neutron diffraction. The promise of neutrons has not changed since the first crystal diffraction data were collected. Today, with the developments of beamlines at spallation neutron sources and the use of the Laue method for data collection, the field of neutrons in structural biology has renewed vitality.

An Inquiry-Based Project Focused on the X-Ray Powder Diffraction Analysis of Common Household Solids

ERIC Educational Resources Information Center

Hulien, Molly L.; Lekse, Jonathan W.; Rosmus, Kimberly A.; Devlin, Kasey P.; Glenn, Jennifer R.; Wisneski, Stephen D.; Wildfong, Peter; Lake, Charles H.; MacNeil, Joseph H.; Aitken, Jennifer A.

2015-01-01

While X-ray powder diffraction (XRPD) is a fundamental analytical technique used by solid-state laboratories across a breadth of disciplines, it is still underrepresented in most undergraduate curricula. In this work, we incorporate XRPD analysis into an inquiry-based project that requires students to identify the crystalline component(s) of…

Using Variable Temperature Powder X-Ray Diffraction to Determine the Thermal Expansion Coefficient of Solid MgO

ERIC Educational Resources Information Center

Corsepius, Nicholas C.; DeVore, Thomas C.; Reisner, Barbara A.; Warnaar, Deborah L.

2007-01-01

A laboratory exercise was developed by using variable temperature powder X-ray diffraction (XRD) to determine [alpha] for MgO (periclase)and was tested in the Applied Physical Chemistry and Materials Characterization Laboratories at James Madison University. The experiment which was originally designed to provide undergraduate students with a…

Analysis of macromolecules, ligands and macromolecule-ligand complexes

DOEpatents

Von Dreele, Robert B [Los Alamos, NM

2008-12-23

A method for determining atomic level structures of macromolecule-ligand complexes through high-resolution powder diffraction analysis and a method for providing suitable microcrystalline powder for diffraction analysis are provided. In one embodiment, powder diffraction data is collected from samples of polycrystalline macromolecule and macromolecule-ligand complex and the refined structure of the macromolecule is used as an approximate model for a combined Rietveld and stereochemical restraint refinement of the macromolecule-ligand complex. A difference Fourier map is calculated and the ligand position and points of interaction between the atoms of the macromolecule and the atoms of the ligand can be deduced and visualized. A suitable polycrystalline sample of macromolecule-ligand complex can be produced by physically agitating a mixture of lyophilized macromolecule, ligand and a solvent.

The Stanford Automated Mounter: Enabling High-Throughput Protein Crystal Screening at SSRL

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

Smith, C.A.; Cohen, A.E.

2009-05-26

The macromolecular crystallography experiment lends itself perfectly to high-throughput technologies. The initial steps including the expression, purification, and crystallization of protein crystals, along with some of the later steps involving data processing and structure determination have all been automated to the point where some of the last remaining bottlenecks in the process have been crystal mounting, crystal screening, and data collection. At the Stanford Synchrotron Radiation Laboratory, a National User Facility that provides extremely brilliant X-ray photon beams for use in materials science, environmental science, and structural biology research, the incorporation of advanced robotics has enabled crystals to be screenedmore » in a true high-throughput fashion, thus dramatically accelerating the final steps. Up to 288 frozen crystals can be mounted by the beamline robot (the Stanford Auto-Mounting System) and screened for diffraction quality in a matter of hours without intervention. The best quality crystals can then be remounted for the collection of complete X-ray diffraction data sets. Furthermore, the entire screening and data collection experiment can be controlled from the experimenter's home laboratory by means of advanced software tools that enable network-based control of the highly automated beamlines.« less

Slow positron applications at slow positron facility of institute of materials structure science, KEK

NASA Astrophysics Data System (ADS)

Hyodo, Toshio; Mochizuki, Izumi; Wada, Ken; Toge, Nobukazu; Shidara, Tetsuo

2018-05-01

Slow Positron Facility at High Energy Accelerator Research Organization (KEK) is a user dedicated facility with an energy-tunable (0.1 - 35 keV) slow positron beam created by a dedicated ˜ 50 MeV linac. It operates in a short pulse (width 1-12 ns, variable, 5×106 e+/s) and a long pulse (width 1.2 µs, 5×107 e+/s) modes of 50 Hz. High energy positrons from pair creation are moderated by reemission after thermalization in W foils. The reemitted positrons are then electrostatically accelerated to a desired energy up to 35 keV and magnetically transported. A pulse-stretching section (pulse stretcher) is installed in the middle of the beamline. It stretches the slow positron pulse for the experiments where too many positrons annihilating in the sample at the same time has to be avoided. Four experiment stations for TRHEPD (total-reflection high-energy positron diffraction), LEPD (low-energy positron diffraction), Ps- (positronium negative ion), and Ps-TOF (positronium time-of-flight) experiments are connected to the beamline branches, SPF-A3, SPF-A4, SPF-B1 and SPF-B2, respectively. Recent results of these stations are briefly described.

Application of Powder Diffraction Methods to the Analysis of the Atomic Structure of Nanocrystals: The Concept of the Apparent Lattice Parameter (ALP)

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Gierlotka, S.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Weber, H.-P.; Palosz, W.; Curreri, Peter A. (Technical Monitor)

2002-01-01

The applicability of standard methods of elaboration of powder diffraction data for determination of the structure of nano-size crystallites is analysed. Based on our theoretical calculations of powder diffraction data we show, that the assumption of the infinite crystal lattice for nanocrystals smaller than 20 nm in size is not justified. Application of conventional tools developed for elaboration of powder diffraction data, like the Rietveld method, may lead to erroneous interpretation of the experimental results. An alternate evaluation of diffraction data of nanoparticles, based on the so-called 'apparent lattice parameter' (alp) is introduced. We assume a model of nanocrystal having a grain core with well-defined crystal structure, surrounded by a surface shell with the atomic structure similar to that of the core but being under a strain (compressive or tensile). The two structural components, the core and the shell, form essentially a composite crystal with interfering, inseparable diffraction properties. Because the structure of such a nanocrystal is not uniform, it defies the basic definitions of an unambiguous crystallographic phase. Consequently, a set of lattice parameters used for characterization of simple crystal phases is insufficient for a proper description of the complex structure of nanocrystals. We developed a method of evaluation of powder diffraction data of nanocrystals, which refers to a core-shell model and is based on the 'apparent lattice parameter' methodology. For a given diffraction pattem, the alp values are calculated for every individual Bragg reflection. For nanocrystals the alp values depend on the diffraction vector Q. By modeling different a0tomic structures of nanocrystals and calculating theoretically corresponding diffraction patterns using the Debye functions we showed, that alp-Q plots show characteristic shapes which can be used for evaluation of the atomic structure of the core-shell system. We show, that using a simple model of a nanocrystal with spherical shape and centro-symmetric strain at the surface shell we obtain theoretical alp-Q values which match very well the alp-Q plots determined experimentally for Sic, GaN, and diamond nanopowders. The theoretical models are defined by the lattice parameter of the grain core, thickness of the surface shell, and the magnitude and distribution of the strain field in the surface shell. According to our calculations, the part of the diffraction pattern measured at relatively low diffraction vectors Q (below 10/angstrom) provides information on the surface strain, whle determination of the lattice parameters in the grain core requires measurements at large Q-values (above 15 - 20/angstrom).

Partially coherent X-ray wavefront propagation simulations including grazing-incidence focusing optics.

PubMed

Canestrari, Niccolo; Chubar, Oleg; Reininger, Ruben

2014-09-01

X-ray beamlines in modern synchrotron radiation sources make extensive use of grazing-incidence reflective optics, in particular Kirkpatrick-Baez elliptical mirror systems. These systems can focus the incoming X-rays down to nanometer-scale spot sizes while maintaining relatively large acceptance apertures and high flux in the focused radiation spots. In low-emittance storage rings and in free-electron lasers such systems are used with partially or even nearly fully coherent X-ray beams and often target diffraction-limited resolution. Therefore, their accurate simulation and modeling has to be performed within the framework of wave optics. Here the implementation and benchmarking of a wave-optics method for the simulation of grazing-incidence mirrors based on the local stationary-phase approximation or, in other words, the local propagation of the radiation electric field along geometrical rays, is described. The proposed method is CPU-efficient and fully compatible with the numerical methods of Fourier optics. It has been implemented in the Synchrotron Radiation Workshop (SRW) computer code and extensively tested against the geometrical ray-tracing code SHADOW. The test simulations have been performed for cases without and with diffraction at mirror apertures, including cases where the grazing-incidence mirrors can be hardly approximated by ideal lenses. Good agreement between the SRW and SHADOW simulation results is observed in the cases without diffraction. The differences between the simulation results obtained by the two codes in diffraction-dominated cases for illumination with fully or partially coherent radiation are analyzed and interpreted. The application of the new method for the simulation of wavefront propagation through a high-resolution X-ray microspectroscopy beamline at the National Synchrotron Light Source II (Brookhaven National Laboratory, USA) is demonstrated.

Dynamic full-field infrared imaging with multiple synchrotron beams

PubMed Central

Stavitski, Eli; Smith, Randy J.; Bourassa, Megan W.; Acerbo, Alvin S.; Carr, G. L.; Miller, Lisa M.

2013-01-01

Microspectroscopic imaging in the infrared (IR) spectral region allows for the examination of spatially resolved chemical composition on the microscale. More than a decade ago, it was demonstrated that diffraction limited spatial resolution can be achieved when an apertured, single pixel IR microscope is coupled to the high brightness of a synchrotron light source. Nowadays, many IR microscopes are equipped with multi-pixel Focal Plane Array (FPA) detectors, which dramatically improve data acquisition times for imaging large areas. Recently, progress been made toward efficiently coupling synchrotron IR beamlines to multi-pixel detectors, but they utilize expensive and highly customized optical schemes. Here we demonstrate the development and application of a simple optical configuration that can be implemented on most existing synchrotron IR beamlines in order to achieve full-field IR imaging with diffraction-limited spatial resolution. Specifically, the synchrotron radiation fan is extracted from the bending magnet and split into four beams that are combined on the sample, allowing it to fill a large section of the FPA. With this optical configuration, we are able to oversample an image by more than a factor of two, even at the shortest wavelengths, making image restoration through deconvolution algorithms possible. High chemical sensitivity, rapid acquisition times, and superior signal-to-noise characteristics of the instrument are demonstrated. The unique characteristics of this setup enabled the real time study of heterogeneous chemical dynamics with diffraction-limited spatial resolution for the first time. PMID:23458231

Entrainment of lactose inhalation powders: a study using laser diffraction.

PubMed

Watling, C P; Elliott, J A; Cameron, R E

2010-07-11

We have investigated the mechanism of entrainment of lactose inhalation blends released from a dry powder inhaler using a diffraction particle size analyser (Malvern Spraytec). Whether a powder blend entrains as a constant stream of powder (the "erosion" mechanism) or as a few coarse plugs (the "fracture" mechanism) was found by comparing transmission data with particle size information. This technique was then applied to a lactose grade with 0, 5 and 10wt% added fine particles. As the wt% fines increased, the entrainment mechanism was found to change from a mild fracture, consisting of multiple small plugs, to more severe fracture with fewer plugs. The most severe fracture mechanism consisted of either the powder reservoir emptying as a single plug, or of the reservoir emptying after a delay of the order of 0.1s due to the powder sticking to its surroundings. Further to this, three different inhalation grades were compared, and the severity of the fracture was found to be inversely proportional to the flowability of the powder (measured using an annular ring shear tester). By considering the volume of aerosolised fine particles in different blends it was determined that the greater the volume of fines added to a powder, the smaller the fraction of fines that were aerosolised. This was attributed to different behaviour when fines disperse from carrier particles compared with when they disperse from agglomerates of fines. In summary, this paper demonstrates how laser diffraction can provide a more detailed analysis of an inhalation powder than just its size distribution. 2010. Published by Elsevier B.V. All rights reserved.

Real-time powder diffraction studies of energy materials under non-equilibrium conditions

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

Peterson, Vanessa K.; Auckett, Josie E.; Pang, Wei-Kong

Energy materials form the central part of energy devices. An essential part of their function is the ability to reversibly host charge or energy carriers, and analysis of their phase composition and structure in real time under non-equilibrium conditions is mandatory for a full understanding of their atomic-scale functional mechanism. Real-time powder diffraction is increasingly being applied for this purpose, forming a critical step in the strategic chemical engineering of materials with improved behaviour. This topical review gives examples of real-time analysis using powder diffraction of rechargeable battery electrodes and porous sorbent materials used for the separation and storage ofmore » energy-relevant gases to demonstrate advances in the insights which can be gained into their atomic-scale function.« less

Real-time powder diffraction studies of energy materials under non-equilibrium conditions

PubMed Central

Peterson, Vanessa K.; Auckett, Josie E.; Pang, Wei-Kong

2017-01-01

Energy materials form the central part of energy devices. An essential part of their function is the ability to reversibly host charge or energy carriers, and analysis of their phase composition and structure in real time under non-equilibrium conditions is mandatory for a full understanding of their atomic-scale functional mechanism. Real-time powder diffraction is increasingly being applied for this purpose, forming a critical step in the strategic chemical engineering of materials with improved behaviour. This topical review gives examples of real-time analysis using powder diffraction of rechargeable battery electrodes and porous sorbent materials used for the separation and storage of energy-relevant gases to demonstrate advances in the insights which can be gained into their atomic-scale function. PMID:28989711

Structural phase transition in d-benzil characterised by capacitance measurements and neutron powder diffraction

NASA Astrophysics Data System (ADS)

Goossens, D. J.; Wu, Xiaodong; Prior, M.

2005-12-01

The ferroelectric phase transition in deuterated benzil, C 14H 10O 2, has been studied using capacitance measurements and neutron powder diffraction. Hydrogenous benzil shows a phase transition at 83.5 K from a high temperature P3 121 phase to a cell-doubled P2 1 phase. The phase transition in d-benzil occurs at 88.1 K, a small isotope effect. Neutron powder diffraction was consistent with a low temperature phase of space group P2 1. Upon deuteration the transition remained first-order and the dynamics of the phenyl ring dominated the behaviour. The isotope effect can be attributed to the difference in mass and moment of inertia between C 6H 5 and C 6D 5.

Synthesis and characterization of Mn-Bi alloy

NASA Astrophysics Data System (ADS)

Mishra, Ashutosh; Patil, Harsha; Jain, G.; Mishra, N.

2012-06-01

High purity MnBi low temperature phase has been prepared and analyzed using X-ray diffraction, Lorentz-Polarization Factor and Fourier transforms infrared measurement. After synthesis of samples structural characterization has done on samples by X-ray diffraction, which shows that after making the bulk sample is in no single phase MnBi has been prepared by sintering Mn and Bi powders. By Lorentz-Polarization Factor is affecting the relative intensity of diffraction lines on a powder form. And by FTIR which shows absorption peaks of MnBi alloys.

Room Temperature Ferromagnetism of Fe Doped Indium Tin Oxide Based on Dispersed Fe3O4 Nanoparticles

NASA Astrophysics Data System (ADS)

Okada, Koichi; Kohiki, Shigemi; Nishi, Sachio; Shimooka, Hirokazu; Deguchi, Hiroyuki; Mitome, Masanori; Bando, Yoshio; Shishido, Toetsu

2007-09-01

Transmission electron microscopy revealed that Fe3O4 nanoparticles with diameter of ≈200 nm dispersed in Fe doped indium tin oxide (Fe@ITO) powders exhibiting co-occurrence of room temperature ferromagnetism and superparamagnetism. Although we observed no X-ray diffraction peak from Fe related compounds for Fe0.19@ITO (ITO: In1.9Sn0.1O3) powders, the powders showed both hysteresis loop in field dependent magnetization at 300 K and divergence of zero-field-cooled magnetization from field-cooled magnetization. Scanning transmission electron microscopy with energy dispersive X-ray spectroscopy demonstrated that the nanoparticle with diameter of ≈200 nm consists of Fe and oxygen. Transmission electron diffraction revealed that crystal structure of the nanoparticle is inverse spinel type Fe3O4. The Fe3O4 crystalline phase by electron diffraction is consistent with the saturation magnetization of 1.3 μB/Fe and magnetic anomaly at ≈110 K observed for the powders.

Controlled nucleation and growth of CdS nanoparticles in a polymer matrix.

PubMed

Di Luccio, Tiziana; Laera, Anna Maria; Tapfer, Leander; Kempter, Susanne; Kraus, Robert; Nickel, Bert

2006-06-29

In-situ synchrotron X-ray diffraction (XRD) was used to monitor the thermal decomposition (thermolysis) of Cd thiolates precursors embedded in a polymer matrix and the nucleation of CdS nanoparticles. A thiolate precursor/polymer solid foil was heated to 300 degrees C in the X-ray diffraction setup of beamline W1.1 at Hasylab, and the diffraction curves were each recorded at 10 degrees C. At temperatures above 240 degrees C, the precursor decomposition is complete and CdS nanoparticles grow within the polymer matrix forming a nanocomposite with interesting optical properties. The nanoparticle structural properties (size and crystal structure) depend on the annealing temperature. Transmission electron microscopy (TEM) and photoluminescence (PL) analyses were used to characterize the nanoparticles. A possible mechanism driving the structural transformation of the precursor is inferred from the diffraction features arising at the different temperatures.

Studies on X-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Miao, Huijie

This dissertation includes three main parts: studies on coherence requirements for the diffraction microscopy experiments, ice formation on frozen-hydrated sample during data collection, and centering of the diffraction data sets. These three subjects are all in support of our groups overall goal of high resolution 3D imaging of frozen hydrated eukaryotic cells via x-ray diffraction microscopy. X-ray diffraction microscopy requires coherent illumination. However, the actual degree of coherence at some beamlines has never been tested. In research on coherence, our first aim is to determine the transverse coherence width at the sample plane at BL 9.0.1 at the Advanced Light Source in Lawrence Berkeley National Laboratory. An analytical calculation of the coherence at the sample plane is presented. Experimental diffraction patterns of pinhole-pair samples were also taken at the beamline to determine the coherence. Due to the irregular shape of the pinholes and other optics complexity, it was very difficult to fit the data with known theoretical equations as it was traditionally done with 1D data. However, we found out that the auto-correlation function shows clearly three spots. Theoretical calculation have been carried out to show that the degree of coherence can be obtained from the intensities of the three spots. These results are compared with the results from the analytical calculation. We then perform a simulation, showing the required transverse coherence width for reconstructing samples with a given size. Ice accumulation has been a major problem in X-ray diffraction microscopy with frozen hydrated samples. Since the ice structure is different from point to point, we cannot subtract the scattering from ice, nor assume a completely "empty" region outside the finite support constraint area as required for reconstruction. Ice forms during the sample preparation and transfer. However, from the tests we did in September 2007, we found that the ice layer thickens significantly during the data collecting process. One of the tests we did was putting a dry room-temperature grid into the beam, cooling it down to liquid nitrogen temperature, and then collecting the diffraction pattern of it over time. This test showed that, after the cold grid remained in the chamber for a while, a ring could be observed in the diffraction pattern. The time necessary for this ring to be visible is highly dependent on the pressure and vacuum history of the chamber. We will discuss how the chamber pressure influences the ice accumulation rate, how an anti-contamination device can help to reduce the rate, and how this ring forms. The last part of the research is based on simulations and a real data set collected on beamline 9.0.1 at the ALS in Berkeley. In X-ray diffraction microscopy, one of the major challenges when processing the data is to accurately determine the true center of the recorded data; that is, the zero spatial frequency position. Simulations of reconstructing shifted data show that if the center of a 2D diffraction pattern is shifted by more than 3 pixels from its true center, the positivity constraint to the phase, which otherwise might be applied to improve the convergence of the reconstruction algorithm, cannot be imposed. Moreover, the phase unwrapping problem may appear during the reconstruction. These issues undermine the quality of the reconstruction of 2D data. Furthermore, the individual shift in each 2D pattern will lead to errors when assembling a 3D diffraction data cube, making the 3D reconstruction very difficult. We developed a method which uses power spectra of the partial diffraction pattern to pre-align the data. A reconstruction without severe phase unwrapping can then be obtained from the pre-aligned data. Next, the precise zero spatial frequency position can be found by examining the linear ramp present in the reconstructed phase. This method was applied to a freeze-dried yeast data set to show that this approach is effective with experimental data.

Structural and Spectral Characterization of Co2+- and Ni2+-DOPED CdO Powder Prepared From Solution at Room Temperature

NASA Astrophysics Data System (ADS)

Reddy, C. V.; Rao, L. V. Krishna; Satish, D. V.; Shim, J.; Ravikumar, R. V. S. S. N.

2015-11-01

The mild and simple solution method was used for the synthesis of Co2+- and Ni2+-doped CdO powders at room temperature. The prepared powders were characterized using powder X-ray diffraction, scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), optical absorption, and Fourier transform infrared spectroscopy (FTIR). From the powder X-ray diffraction patterns, it has been observed that the prepared Co2+ and Ni2+ ion-doped CdO powders belong to the cubic phase, and the evaluated average crystalline sizes of the powders are 20 and 14 nm, respectively. The SEM images and the EDS spectra show that the prepared powders are distributed over different sizes in the grain boundaries. Optical absorption studies allow determination of site symmetry of the metal ion with its ligands. The crystal field (Dq) and inter-electronic repulsion (B and C) parameters have been evaluated from the optical absorption spectra. The FTIR spectra show the characteristic fundamental vibrations of the metal oxide and CdO.

Applications of X-Ray Micro-Beam for Data Collection.

PubMed

Sanishvili, Ruslan; Fischetti, Robert F

2017-01-01

Micro-diffraction tools for macromolecular crystallography, first developed at the end of 1990s and now an integral part of many synchrotron beamlines, enable some of the experiments which were not feasible just a decade or so ago. These include data collection from very small samples, just a few micrometers in size; from larger, but severely inhomogeneous samples; and from samples which are optically invisible. Improved micro-diffraction tools led to improved signal-to-noise ratio, to mitigation of radiation damage in some cases, and to better-designed diffraction experiments. Small, micron-scale beams can be attained in different ways and knowing the details of the implementation is important in order to design the diffraction experiment properly. Similarly, precision, reproducibility and stability of the goniometry, and caveats of detection systems need to be taken into account. Lastly, to make micro-diffraction widely applicable, the sophistication, robustness, and user-friendliness of these tools are just as important as the technical capabilities.

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

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

Fan, D.; Luo, S. N., E-mail: sluo@pims.ac.cn; Key Laboratory of Advanced Technologies of Materials, Ministry of Education, Southwest Jiaotong University, Chengdu, Sichuan 610031

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; fracture is dominated by splitting cracks followed by wing cracks, and diffraction peaks are broadened likely due to mosaic spread. Our results demonstrate the potential of such multiscale measurements for studying high strain-rate phenomena at dynamic extremes.« less

Synchrotron FTIR Imaging For The Identification Of Cell Types Within Human Tissues

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

Walsh, Michael J.; Pounder, F. Nell; Nasse, Michael J.

2010-02-03

The use of synchrotron Fourier Transform Infrared spectroscopy (S-FTIR) has been shown to be a very promising tool for biomedical research. S-FTIR spectroscopy allows for the fast acquisition of infrared (IR) spectra at a spatial resolution approaching the IR diffraction limit. The development of the Infrared Environmental Imaging (IRENI) beamline at the Synchrotron Radiation Center (SRC) at the University of Wisconsin-Madison has allowed for diffraction limited imaging measurements of cells in human prostate and breast tissues. This has allowed for the identification of cell types within tissues that would otherwise not have been resolvable using conventional FTIR sources.

Performance of multilayer coated diffraction gratings in the EUV

NASA Technical Reports Server (NTRS)

Keski-Kuha, Ritva A. M.; Thomas, Roger J.; Gum, Jeffrey S.; Condor, Charles E.

1990-01-01

The effect of multilayer coating application on the performance of a diffraction grating in the EUV spectral region was evaluated by examining the performance of a 3600-line/mm and a 1200-line/mm replica blazed gratings, designed for operation in the 300-A spectral region in first order. A ten-layer IrSi multilayer optimized for 304 A was deposited using electron-beam evaporation. The grating efficiency was measured on the SURF II calibration beamline in a chamber designed for calibrating the solar EUV rocket telescope and spectrograph multilayer coatings. A significant (by a factor of about 7) enhancement in grating efficiency in the 300-A region was demonstrated.

Micro-crystallography comes of age

PubMed Central

Smith, Janet L.; Fischetti, Robert F.; Yamamoto, Masaki

2012-01-01

The latest revolution in macromolecular crystallography was incited by the development of dedicated, user friendly, micro-crystallography beamlines. Brilliant X-ray beams of diameter 20 microns or less, now available at most synchrotron sources, enable structure determination from samples that previously were inaccessible. Relative to traditional crystallography, crystals with one or more small dimensions have diffraction patterns with vastly improved signal-to-noise when recorded with an appropriately matched beam size. Structures can be solved from isolated, well diffracting regions within inhomogeneous samples. This review summarizes the technological requirements and approaches to producing micro-beams and how they continue to change the practice of crystallography. PMID:23021872

Diffraction enhance x-ray imaging for quantitative phase contrast studies

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

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

2016-05-23

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

Acoustic methods for high-throughput protein crystal mounting at next-generation macromolecular crystallographic beamlines.

PubMed

Roessler, Christian G; Kuczewski, Anthony; Stearns, Richard; Ellson, Richard; Olechno, Joseph; Orville, Allen M; Allaire, Marc; Soares, Alexei S; Héroux, Annie

2013-09-01

To take full advantage of advanced data collection techniques and high beam flux at next-generation macromolecular crystallography beamlines, rapid and reliable methods will be needed to mount and align many samples per second. One approach is to use an acoustic ejector to eject crystal-containing droplets onto a solid X-ray transparent surface, which can then be positioned and rotated for data collection. Proof-of-concept experiments were conducted at the National Synchrotron Light Source on thermolysin crystals acoustically ejected onto a polyimide `conveyor belt'. Small wedges of data were collected on each crystal, and a complete dataset was assembled from a well diffracting subset of these crystals. Future developments and implementation will focus on achieving ejection and translation of single droplets at a rate of over one hundred per second.

Acoustic methods for high-throughput protein crystal mounting at next-generation macromolecular crystallographic beamlines

PubMed Central

Roessler, Christian G.; Kuczewski, Anthony; Stearns, Richard; Ellson, Richard; Olechno, Joseph; Orville, Allen M.; Allaire, Marc; Soares, Alexei S.; Héroux, Annie

2013-01-01

To take full advantage of advanced data collection techniques and high beam flux at next-generation macromolecular crystallography beamlines, rapid and reliable methods will be needed to mount and align many samples per second. One approach is to use an acoustic ejector to eject crystal-containing droplets onto a solid X-ray transparent surface, which can then be positioned and rotated for data collection. Proof-of-concept experiments were conducted at the National Synchrotron Light Source on thermolysin crystals acoustically ejected onto a polyimide ‘conveyor belt’. Small wedges of data were collected on each crystal, and a complete dataset was assembled from a well diffracting subset of these crystals. Future developments and implementation will focus on achieving ejection and translation of single droplets at a rate of over one hundred per second. PMID:23955046

X-ray diffraction studies of shocked lunar analogs

NASA Technical Reports Server (NTRS)

Hanss, R. E.

1979-01-01

The X-ray diffraction experiments on shocked rock and mineral analogs of particular significance to lunar geology are described. Materials naturally shocked by meteorite impact, nuclear-shocked, or artificially shocked in a flat plate accelerator were utilized. Four areas were outlined for investigation: powder diffractometer studies of shocked single crystal silicate minerals (quartz, orthoclase, oligoclase, pyroxene), powder diffractometer studies of shocked polycrystalline monomineralic samples (dunite), Debye-Scherrer studies of single grains of shocked granodiorite, and powder diffractometer studies of shocked whole rock samples. Quantitative interpretation of peak shock pressures experienced by materials found in lunar or terrestrial impact structures is presented.

The life science X-ray scattering beamline at NSLS-II

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

DiFabio, Jonathan; Yang, Lin; Chodankar, Shirish

We report the current development status of the High Brightness X-ray Scattering for Life Sciences (or Life Science X-ray Scattering, LiX) beamline at the NSLS-II facility of Brookhaven National Laboratory. This instrument will operate in the x-ray energy range of 2.1-18 keV, provide variable beam sizes from 1 micron to ~0.5 mm, and support user experiments in three scientific areas: (1) high-throughput solution scattering, in-line size exclusion chromatography and flow mixers-based time-resolved solution scattering of biological macro-molecules, (2) diffraction from single- and multi-layered lipid membranes, and (3) scattering-based scanning probe imaging of biological tissues. In order to satisfy the beammore » stability required for these experiments and to switch rapidly between different types of experiments, we have adopted a secondary source with refractive lenses for secondary focusing, a detector system consisting of three Pilatus detectors, and specialized experimental modules that can be quickly exchanged and each dedicated to a defined set of experiments. The construction of this beamline is on schedule for completion in September 2015. User experiments are expected to start in Spring 2016.« less

The life science X-ray scattering beamline at NSLS-II

DOE PAGES

DiFabio, Jonathan; Yang, Lin; Chodankar, Shirish; ...

2015-09-30

We report the current development status of the High Brightness X-ray Scattering for Life Sciences (or Life Science X-ray Scattering, LiX) beamline at the NSLS-II facility of Brookhaven National Laboratory. This instrument will operate in the x-ray energy range of 2.1-18 keV, provide variable beam sizes from 1 micron to ~0.5 mm, and support user experiments in three scientific areas: (1) high-throughput solution scattering, in-line size exclusion chromatography and flow mixers-based time-resolved solution scattering of biological macro-molecules, (2) diffraction from single- and multi-layered lipid membranes, and (3) scattering-based scanning probe imaging of biological tissues. In order to satisfy the beammore » stability required for these experiments and to switch rapidly between different types of experiments, we have adopted a secondary source with refractive lenses for secondary focusing, a detector system consisting of three Pilatus detectors, and specialized experimental modules that can be quickly exchanged and each dedicated to a defined set of experiments. The construction of this beamline is on schedule for completion in September 2015. User experiments are expected to start in Spring 2016.« less

The life science x-ray scattering beamline at NSLS-II

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

DiFabio, Jonathan; Chodankar, Shirish; Pjerov, Sal

We report the current development status of the High Brightness X-ray Scattering for Life Sciences (or Life Science X-ray Scattering, LiX) beamline at the NSLS-II facility of Brookhaven National Laboratory. This instrument will operate in the x-ray energy range of 2.1-18 keV, provide variable beam sizes from 1 micron to ∼0.5 mm, and support user experiments in three scientific areas: (1) high-throughput solution scattering, in-line size exclusion chromatography and flow mixers-based time-resolved solution scattering of biological macro-molecules, (2) diffraction from single- and multi-layered lipid membranes, and (3) scattering-based scanning probe imaging of biological tissues. In order to satisfy the beammore » stability required for these experiments and to switch rapidly between different types of experiments, we have adopted a secondary source with refractive lenses for secondary focusing, a detector system consisting of three Pilatus detectors, and specialized experimental modules that can be quickly exchanged and each dedicated to a defined set of experiments. The construction of this beamline is on schedule for completion in September 2015. User experiments are expected to start in Spring 2016.« less

Simulation and optimization of the SIRIUS IPE soft x-ray beamline

NASA Astrophysics Data System (ADS)

Meyer, Bernd C.; Rocha, Tulio C. R.; Luiz, Sergio A. L.; C. Pinto, Artur; Westfahl, Harry

2017-08-01

The soft X-ray beamline IPE is one of the first phase SIRIUS beamlines at the LNLS, Brazil. Divided into two branches, IPE is designed to perform ambient pressure X-ray photo-electron spectroscopy (AP-XPS) and high resolution resonant inelastic X-ray scattering (RIXS) for samples in operando/environmental conditions inside cells and liquid jets. The aim is to maximize the photon flux in the energy range 200-1400 eV generated by an elliptically polarizing undulator source (EPU) and focus it to a 1 μm vertical spot size at the RIXS station and 10 μm at the AP-XPS station. In order to achieve the required resolving power (40.000 at 930 eV) for RIXS both the dispersion properties of the plane grating monochromator (PGM) and the thermal deformation of the optical elements need special attention. The grating parameters were optimized with the REFLEC code to maximize the efficiency at the required resolution. Thermal deformation of the PGM plane mirror limits the possible range of cff parameters depending of the photon energy used. Hence, resolution of the PGM and thermal deformation effects define the boundary conditions of the optical concept and the simulations of the IPE beamline. We compare simulations performed by geometrical ray-tracing (SHADOW) and wave front propagation (SRW) and show that wave front diffraction effects (apertures, optical surface error profiles) has a small effect on the beam spot size and shape.

On the possibility of using polycrystalline material in the development of structure-based generic assays

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

Allaire, Marc, E-mail: allaire@bnl.gov; Moiseeva, Natalia; Botez, Cristian E.

The correlation coefficients calculated between raw powder diffraction profiles can be used to identify ligand-bound/unbound states of lysozyme. The discovery of ligands that bind specifically to a targeted protein benefits from the development of generic assays for high-throughput screening of a library of chemicals. Protein powder diffraction (PPD) has been proposed as a potential method for use as a structure-based assay for high-throughput screening applications. Building on this effort, powder samples of bound/unbound states of soluble hen-egg white lysozyme precipitated with sodium chloride were compared. The correlation coefficients calculated between the raw diffraction profiles were consistent with the known bindingmore » properties of the ligands and suggested that the PPD approach can be used even prior to a full description using stereochemically restrained Rietveld refinement.« less

Addressing the amorphous content issue in quantitative phase analysis: the certification of NIST standard reference material 676a.

PubMed

Cline, James P; Von Dreele, Robert B; Winburn, Ryan; Stephens, Peter W; Filliben, James J

2011-07-01

A non-diffracting surface layer exists at any boundary of a crystal and can comprise a mass fraction of several percent in a finely divided solid. This has led to the long-standing issue of amorphous content in standards for quantitative phase analysis (QPA). NIST standard reference material (SRM) 676a is a corundum (α-Al(2)O(3)) powder, certified with respect to phase purity for use as an internal standard in powder diffraction QPA. The amorphous content of SRM 676a is determined by comparing diffraction data from mixtures with samples of silicon powders that were engineered to vary their specific surface area. Under the (supported) assumption that the thickness of an amorphous surface layer on Si was invariant, this provided a method to control the crystalline/amorphous ratio of the silicon components of 50/50 weight mixtures of SRM 676a with silicon. Powder diffraction experiments utilizing neutron time-of-flight and 25 keV and 67 keV X-ray energies quantified the crystalline phase fractions from a series of specimens. Results from Rietveld analyses, which included a model for extinction effects in the silicon, of these data were extrapolated to the limit of zero amorphous content of the Si powder. The certified phase purity of SRM 676a is 99.02% ± 1.11% (95% confidence interval). This novel certification method permits quantification of amorphous content for any sample of interest, by spiking with SRM 676a.

APS Science 2006.

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

Gibson, J. M.; Fenner, R. B.; Long, G.

2007-05-24

In my five years as the Director of the Advanced Photon Source (APS), I have been fortunate to see major growth in the scientific impact from the APS. This year I am particularly enthusiastic about prospects for our longer-term future. Every scientific instrument must remain at the cutting edge to flourish. Our plans for the next generation of APS--an APS upgrade--got seriously in gear this year with strong encouragement from our users and sponsors. The most promising avenue that has emerged is the energy-recovery linac (ERL) (see article on page xx), for which we are beginning serious R&D. The ERL{at}APSmore » would offer revolutionary performance, especially for x-ray imaging and ultrafast science, while not seriously disrupting the existing user base. I am very proud of our accelerator physics and engineering staff, who not only keep the current APS at the forefront, but were able to greatly impress our international Machine Advisory Committee with the quality of their work on the possible upgrade option (see page xx). As we prepare for long-term major upgrades, our plans to develop and optimize all the sectors at APS in the near future are advancing. Several new beamlines saw first light this year, including a dedicated powder diffraction beamline (11-BM), two instruments for inelastic x-ray scattering at sector 30, and the Center for Nanoscale Materials (CNM) Nanoprobe beamline at sector 26. Our partnership in the first x-ray free-electron laser (LCLS) to be built at Stanford contributes to revolutionary growth in ultrafast science (see page xx), and we are developing a pulse chirping scheme to get ps pulses at sector 7 of the APS within a year or so. In this report, you will find selected highlights of scientific research at the APS from calendar year 2006. The highlighted work covers diverse disciplines, from fundamental to applied science. In the article on page xx you can see the direct impact of APS research on technology. Several new products have emerged from work at the APS, to complement the tremendous output of work in basic science, which often has payoff in technology but over decades rather than years. Highlights in this report also reflect the relevance of APS work to Department of Energy missions, for example a route to more efficient fuel cells (page xx mr-88-073113) addresses the energy challenge, and natural approaches to cleaning up the environment.« less

Effect of the Chemical State of the Surface on the Relaxation of the Surface Shell Atoms in SiC and GaN Nanocrystals

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Weber, H. P.; Janik, J. F.; Palosz, W.; Curreri, Peter A. (Technical Monitor)

2002-01-01

The effect of the chemical state of the surface of nanoparticles on the relaxation in the near-surface layer was examined using the concept of the apparent lattice parameter (alp) determined for different diffraction vectors Q. The apparent lattice parameter is a lattice parameter determined either from an individual Bragg reflection, or from a selected region of the diffraction pattern. At low diffraction vectors the Bragg peak positions are affected mainly by the structure of the near-surface layer, while at high Q-values only the interior of the nano-grain contributes to the diffraction pattern. Following the measurements on raw (as prepared) powders we investigated powders cleaned by annealing at 400C under vacuum, and the same powders wetted with water. Theoretical alp-Q plots showed that the structure of the surface layer depends on the sample treatment. Semi-quantitative analysis based on the comparison of the experimental and theoretical alp-Q plots was performed. Theoretical alp-Q relations were obtained from the diffraction patterns calculated for models of nanocrystals with a strained surface layer using the Debye functions.

Characterization of composite materials based on cement-ceramic powder blended binder

NASA Astrophysics Data System (ADS)

Kulovaná, Tereza; Pavlík, Zbyšek

2016-06-01

Characterization of newly developed composite mortars with incorporated ceramic powder coming from precise brick cutting as partial Portland cement replacement up to 40 mass% is presented in the paper. Fine ceramic powder belongs to the pozzolanic materials. Utilization of pozzolanic materials is accompanied by lower request on energy needed for Portland clinker production which generally results in lower production costs of blended binder and lower CO2 emission. In this paper, the ceramic powder is used in cement based mortar composition in amount of 8, 16, 24, 32, and 40 mass% of cement. Chemical composition of ceramic powder is analyzed by X-Ray Fluorescence and X-Ray Diffraction. The particle size distribution of ceramics is accessed on laser diffraction principle. For 28 days cured mortar samples, basic physical and mechanical properties are experimentally determined. The obtained results demonstrate that ceramic powder has potential to replace a part of Portland cement in composition of cement based composites and to reduce negative environmental impact of their production.

Phase analysis of ZrO2-SiO2 systems synthesized through Ball milling mechanical activations

NASA Astrophysics Data System (ADS)

Nurlaila, Rizka; Musyarofah, Muwwaqor, Nibras Fuadi; Triwikantoro, Kuswoyo, Anton; Pratapa, Suminar

2017-01-01

Zircon powders have been produced from raw materials of amorphous zirconia and amorphous silica powders obtained from natural zircon sand of Kalimantan Tengah, Indonesia. Synthesis process was started with the extraction of zircon powder to produce sodium silicate solution and pure zircon powder. The amorphous zirconia and silica powders were prepared by alkali fusion and co-precipitation techniques. The powders were mixed using a planetary ball mill, followed by a calcination of various holding time of 3, 10, and 15 h. Phase characterization was done using X-Ray Diffraction (XRD) technique and analysis of the diffraction data was carried out using Rietica and MAUD software. The identified phases after the calcination were zircon, tetragonal zirconia, and cristobalite. The highest zircon content was obtained in the sample calcinated for15 hours - reaching 99.66 %wt. Crystallite size analysis revealed that the samples calcinated for 3, 10, and 15 h exhibited zircon crystal size of 176 (1) nm, 191 (1) nm and 233 (1) nm respectively.

Characterization of composite materials based on cement-ceramic powder blended binder

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

Kulovaná, Tereza; Pavlík, Zbyšek

Characterization of newly developed composite mortars with incorporated ceramic powder coming from precise brick cutting as partial Portland cement replacement up to 40 mass% is presented in the paper. Fine ceramic powder belongs to the pozzolanic materials. Utilization of pozzolanic materials is accompanied by lower request on energy needed for Portland clinker production which generally results in lower production costs of blended binder and lower CO{sub 2} emission. In this paper, the ceramic powder is used in cement based mortar composition in amount of 8, 16, 24, 32, and 40 mass% of cement. Chemical composition of ceramic powder is analyzedmore » by X-Ray Fluorescence and X-Ray Diffraction. The particle size distribution of ceramics is accessed on laser diffraction principle. For 28 days cured mortar samples, basic physical and mechanical properties are experimentally determined. The obtained results demonstrate that ceramic powder has potential to replace a part of Portland cement in composition of cement based composites and to reduce negative environmental impact of their production.« less

Performance Characteristics of Waste Glass Powder Substituting Portland Cement in Mortar Mixtures

NASA Astrophysics Data System (ADS)

Kara, P.; Csetényi, L. J.; Borosnyói, A.

2016-04-01

In the present work, soda-lime glass cullet (flint, amber, green) and special glass cullet (soda-alkaline earth-silicate glass coming from low pressure mercury-discharge lamp cullet and incandescent light bulb borosilicate glass waste cullet) were ground into fine powders in a laboratory planetary ball mill for 30 minutes. CEM I 42.5N Portland cement was applied in mortar mixtures, substituted with waste glass powder at levels of 20% and 30%. Characterisation and testing of waste glass powders included fineness by laser diffraction particle size analysis, specific surface area by nitrogen adsorption technique, particle density by pycnometry and chemical analysis by X-ray fluorescence spectrophotometry. Compressive strength, early age shrinkage cracking and drying shrinkage tests, heat of hydration of mortars, temperature of hydration, X-ray diffraction analysis and volume stability tests were performed to observe the influence of waste glass powder substitution for Portland cement on physical and engineering properties of mortar mixtures.

Fabrication, characterization and fracture study of a machinable hydroxyapatite ceramic.

PubMed

Shareef, M Y; Messer, P F; van Noort, R

1993-01-01

In this study the preparation of a machinable hydroxyapatite from mixtures of a fine, submicrometer powder and either a coarse powder composed of porous aggregates up to 50 microns or a medium powder composed of dense particles of 3 microns median size is described. These were characterized using X-ray diffraction, transmission and scanning electron microscopy and infra-red spectroscopy. Test-pieces were formed by powder pressing and slip casting mixtures of various combinations of the fine, medium and coarse powders. The fired test-pieces were subjected to measurements of firing shrinkage, porosity, bulk density, tensile strength and fracture toughness. The microstructure and composition were examined using scanning electron microscopy and X-ray diffraction. For both processing methods, a uniform interconnected microporous structure was produced of a high-purity hydroxyapatite. The maximum tensile strength and fracture toughness that could be attained while retaining machinability were 37 MPa and 0.8 MPa m1/2 respectively.

Polymorphism of Alprazolam (Xanax): a review of its crystalline phases and identification, crystallographic characterization, and crystal structure of a new polymorph (form III).

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Van den Mooter, Guy; Blaton, Norbert

2007-05-01

A new polymorphic form of Alprazolam (Xanax), 8-chloro-1-methyl-6-phenyl-4H-[1,2,4]triazolo-[4,3-alpha][1,4]benzodiazepine, C(17)H(13)ClN(4), has been investigated by means of X-ray powder diffraction (XRPD), single crystal X-ray diffraction, and differential scanning calorimetry (DSC). This polymorphic form (form III) was obtained during DSC experiments after the exothermic recrystallization of the melt of form I. The crystal unit cell dimensions for form III were determined from diffractometer methods. The monoclinic unit cell found for this polymorph using XRPD after indexing the powder diffractogram was confirmed by the cell parameters obtained from single crystal X-ray diffractometry on a crystal isolated from the DSC pans. The single crystal unit cell parameters are: a = 28.929(9), b = 13.844(8), c = 7.361(3) angstroms, beta = 92.82(3) degrees , V = 2944(2) angstroms(3), Z = 8, space group P2(1) (No.4), Dx = 1.393 Mg/m(3). The structure obtained from single crystal X-ray diffraction was used as initial model for Rietveld refinement on the powder diffraction data of form III. The temperature phase transformations of alprazolam were also studied using high temperature XRPD. A review of the different phases available in the Powder Diffraction File (PDF) database for this drug is described bringing some clarification and corrections. (c) 2007 Wiley-Liss, Inc. and the American Pharmacists Association.

Mg(1 + x)Ir(1 - x) (x = 0, 0.037 and 0.054), a binary intermetallic compound with a new orthorhombic structure type determined from powder and single-crystal X-ray diffraction.

PubMed

Cerný, Radovan; Renaudin, Guillaume; Favre-Nicolin, Vincent; Hlukhyy, Viktor; Pöttgen, Rainer

2004-06-01

The new binary compound Mg(1 + x)Ir(1 - x) (x = 0-0.054) was prepared by melting the elements in the Mg:Ir ratio 2:3 in a sealed tantalum tube under an argon atmosphere in an induction furnace (single crystals) or by annealing cold-pressed pellets of the starting composition Mg:Ir 1:1 in an autoclave under an argon atmosphere (powder sample). The structure was independently solved from high-resolution synchrotron powder and single-crystal X-ray data: Pearson symbol oC304, space group Cmca, lattice parameters from synchrotron powder data a = 18.46948 (6), b = 16.17450 (5), c = 16.82131 (5) A. Mg(1 + x)Ir(1 - x) is a topologically close-packed phase, containing 13 Ir and 12 Mg atoms in the asymmetric unit, and has a narrow homogeneity range. Nearly all the atoms have Frank-Kasper-related coordination polyhedra, with the exception of two Ir atoms, and this compound contains the shortest Ir-Ir distances ever observed. The solution of a rather complex crystal structure from powder diffraction, which was fully confirmed by the single-crystal method, shows the power of powder diffraction in combination with the high-resolution data and the global optimization method.

Roller compaction of different pseudopolymorphic forms of theophylline: Effect on compressibility and tablet properties.

PubMed

Hadzović, Ervina; Betz, Gabriele; Hadzidedić, Seherzada; El-Arini, Silvia Kocova; Leuenberger, Hans

2010-08-30

The effect of roller compaction on disintegration time, dissolution rate and compressibility of tablets prepared from theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate was studied. In addition, the influence of adding microcrystalline cellulose, a commonly used excipient, in mixtures with these materials was investigated. Theophylline anhydrate powder was used as a model drug to investigate the influence of different compaction pressures on the tablet properties. Tablets with same porosity were prepared by direct compaction and by roller compaction/re-compaction. Compressibility was characterized by Heckel and modified Heckel equations. Due to the property of polymorphic materials to change their form during milling and compression, X-ray diffraction analysis of theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate powders and granules was carried out. After roller compaction the disintegration time and the dissolution rate of the tablets were significantly improved. Compressibility of theophylline anhydrate powder and theophylline anhydrate fine powder was decreased, while theophylline monohydrate showed higher compressibility after roller compaction. Microcrystalline cellulose affected compressibility of theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate whereby the binary mixtures showed higher compressibility than the individual materials. X-ray diffraction analyses confirmed that there were no polymorphic/pseudopolymorphic changes after roller compaction. Copyright 2010 Elsevier B.V. All rights reserved.

Black Pine Circle Project

ScienceCinema

Mytko, Christine

2018-05-18

A group of seventh graders from Black Pine Circle school in Berkeley had the opportunity to experience the Advanced Light Source (ALS) as "users" via a collaborative field trip and proposal project. The project culminated with a field trip to the ALS for all seventh graders, which included a visit to the ALS data visualization room, a diffraction demonstration, a beamline tour, and informative sessions about x-rays and tomography presented by ALS scientists.

Black Pine Circle Project

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

Mytko, Christine

2014-03-31

A group of seventh graders from Black Pine Circle school in Berkeley had the opportunity to experience the Advanced Light Source (ALS) as "users" via a collaborative field trip and proposal project. The project culminated with a field trip to the ALS for all seventh graders, which included a visit to the ALS data visualization room, a diffraction demonstration, a beamline tour, and informative sessions about x-rays and tomography presented by ALS scientists.

Expression, purification, crystallization and initial crystallographic characterization of the p-hydroxybenzoate hydroxylase from Corynebacterium glutamicum

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

Kwon, Soo-Young; Kang, Beom Sik; Kim, Ghyung-Hwa

2007-11-01

PHBH from Corynebacterium glutamicum was crystallized using the hanging-drop vapour-diffusion method in the presence of NaH{sub 2}PO{sub 4} and K{sub 2}HPO{sub 4} as precipitants. X-ray diffraction data were collected to a maximum resolution of 2.5 Å on a synchrotron beamline. p-Hydroxybenzoate hydroxylase (PHBH) is an FAD-dependent monooxygenase that catalyzes the hydroxylation of p-hydroxybenzoate (pOHB) to 3,4-dihydroxybenzoate in an NADPH-dependent reaction and plays an important role in the biodegradation of aromatic compounds. PHBH from Corynebacterium glutamicum was crystallized using the hanging-drop vapour-diffusion method in the presence of NaH{sub 2}PO{sub 4} and K{sub 2}HPO{sub 4} as precipitants. X-ray diffraction data were collectedmore » to a maximum resolution of 2.5 Å on a synchrotron beamline. The crystal belongs to the hexagonal space group P6{sub 3}22, with unit-cell parameters a = b = 94.72, c = 359.68 Å, γ = 120°. The asymmetric unit contains two molecules, corresponding to a packing density of 2.65 Å{sup 3} Da{sup −1}. The structure was solved by molecular replacement. Structure refinement is in progress.« less

Beam modulation: A novel ToF-technique for high resolution diffraction at the Beamline for European Materials Engineering Research (BEER)

NASA Astrophysics Data System (ADS)

Rouijaa, M.; Kampmann, R.; Šaroun, J.; Fenske, J.; Beran, P.; Müller, M.; Lukáš, P.; Schreyer, A.

2018-05-01

The Beamline for European Materials Engineering Research (BEER) is under construction at the European Spallation Source (ESS) in Lund, Sweden. A basic requirement on BEER is to make best use of the long ESS pulse (2.86 ms) for engineering investigations. High-resolution diffraction, however, demands timing resolution up to 0.1% corresponding to a pulse length down to about 70 μs for the case of thermal neutrons (λ ∼ 1.8 Å). Such timing resolution can be achieved by pulse shaping techniques cutting a short section out of the long pulse, and thus paying for resolution by strong loss of intensity. In contrast to this, BEER proposes a novel operation mode called pulse modulation technique based on a new chopper design, which extracts several short pulses out of the long ESS pulse, and hence leads to a remarkable gain of intensity compared to nowadays existing conventional pulse shaping techniques. The potential of the new technique can be used with full advantage for investigating strains and textures of highly symmetric materials. Due to its instrument design and the high brilliance of the ESS pulse, BEER is expected to become the European flagship for engineering research for strain mapping and texture analysis.

Crystal structure of hydrocortisone acetate, C23H32O6

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

Kaduk, James A.; Gindhart, Amy M.; Blanton, Thomas N.

The crystal structure of hydrocortisone acetate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Hydrocortisone acetate crystallizes in space groupP2 1(#4) witha= 8.85173(3) Å,b= 13.53859(3) Å,c= 8.86980(4) Å,β= 101.5438(3)°,V= 1041.455(6) Å 3, andZ= 2. Both hydroxyl groups form hydrogen bonds to the ketone oxygen atom on the steroid ring system, resulting in a three-dimensional hydrogen bond network. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™.

A dedicated superbend x-ray microdiffraction beamline for materials, geo-, and environmental sciences at the advanced light source.

PubMed

Kunz, Martin; Tamura, Nobumichi; Chen, Kai; MacDowell, Alastair A; Celestre, Richard S; Church, Matthew M; Fakra, Sirine; Domning, Edward E; Glossinger, James M; Kirschman, Jonathan L; Morrison, Gregory Y; Plate, Dave W; Smith, Brian V; Warwick, Tony; Yashchuk, Valeriy V; Padmore, Howard A; Ustundag, Ersan

2009-03-01

A new facility for microdiffraction strain measurements and microfluorescence mapping has been built on beamline 12.3.2 at the advanced light source of the Lawrence Berkeley National Laboratory. This beamline benefits from the hard x-radiation generated by a 6 T superconducting bending magnet (superbend). This provides a hard x-ray spectrum from 5 to 22 keV and a flux within a 1 microm spot of approximately 5x10(9) photons/s (0.1% bandwidth at 8 keV). The radiation is relayed from the superbend source to a focus in the experimental hutch by a toroidal mirror. The focus spot is tailored by two pairs of adjustable slits, which serve as secondary source point. Inside the lead hutch, a pair of Kirkpatrick-Baez (KB) mirrors placed in a vacuum tank refocuses the secondary slit source onto the sample position. A new KB-bending mechanism with active temperature stabilization allows for more reproducible and stable mirror bending and thus mirror focusing. Focus spots around 1 microm are routinely achieved and allow a variety of experiments, which have in common the need of spatial resolution. The effective spatial resolution (approximately 0.2 microm) is limited by a convolution of beam size, scan-stage resolution, and stage stability. A four-bounce monochromator consisting of two channel-cut Si(111) crystals placed between the secondary source and KB-mirrors allows for easy changes between white-beam and monochromatic experiments while maintaining a fixed beam position. High resolution stage scans are performed while recording a fluorescence emission signal or an x-ray diffraction signal coming from either a monochromatic or a white focused beam. The former allows for elemental mapping, whereas the latter is used to produce two-dimensional maps of crystal-phases, -orientation, -texture, and -strain/stress. Typically achieved strain resolution is in the order of 5x10(-5) strain units. Accurate sample positioning in the x-ray focus spot is achieved with a commercial laser-triangulation unit. A Si-drift detector serves as a high-energy-resolution (approximately 150 eV full width at half maximum) fluorescence detector. Fluorescence scans can be collected in continuous scan mode with up to 300 pixels/s scan speed. A charge coupled device area detector is utilized as diffraction detector. Diffraction can be performed in reflecting or transmitting geometry. Diffraction data are processed using XMAS, an in-house written software package for Laue and monochromatic microdiffraction analysis.

A comparative study of the use of powder X-ray diffraction, Raman and near infrared spectroscopy for quantification of binary polymorphic mixtures of piracetam.

PubMed

Croker, Denise M; Hennigan, Michelle C; Maher, Anthony; Hu, Yun; Ryder, Alan G; Hodnett, Benjamin K

2012-04-07

Diffraction and spectroscopic methods were evaluated for quantitative analysis of binary powder mixtures of FII(6.403) and FIII(6.525) piracetam. The two polymorphs of piracetam could be distinguished using powder X-ray diffraction (PXRD), Raman and near-infrared (NIR) spectroscopy. The results demonstrated that Raman and NIR spectroscopy are most suitable for quantitative analysis of this polymorphic mixture. When the spectra are treated with the combination of multiplicative scatter correction (MSC) and second derivative data pretreatments, the partial least squared (PLS) regression model gave a root mean square error of calibration (RMSEC) of 0.94 and 0.99%, respectively. FIII(6.525) demonstrated some preferred orientation in PXRD analysis, making PXRD the least preferred method of quantification. Copyright © 2012 Elsevier B.V. All rights reserved.

Purification, crystallization and preliminary X-ray diffraction analysis of GatD, a glutamine amidotransferase-like protein from Staphylococcus aureus peptidoglycan

PubMed Central

Vieira, Diana; Figueiredo, Teresa A.; Verma, Anil; Sobral, Rita G.; Ludovice, Ana M.; de Lencastre, Hermínia; Trincao, Jose

2014-01-01

Amidation of peptidoglycan is an essential feature in Staphylococcus aureus that is necessary for resistance to β-lactams and lysozyme. GatD, a 27 kDa type I glutamine amidotransferase-like protein, together with MurT ligase, catalyses the amidation reaction of the glutamic acid residues of the peptidoglycan of S. aureus. The native and the selenomethionine-derivative proteins were crystallized using the sitting-drop vapour-diffusion method with polyethylene glycol, sodium acetate and calcium acetate. The crystals obtained diffracted beyond 1.85 and 2.25 Å, respectively, and belonged to space group P212121. X-ray diffraction data sets were collected at Diamond Light Source (on beamlines I02 and I04) and were used to obtain initial phases. PMID:24817726

Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

DOE PAGES

Wang, H.; Kirkham, M. J.; Watkins, T. R.; ...

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

Synthesis of cerium oxide (CeO 2) by co-precipitation for application as a reference material for X-ray powder diffraction peak widths

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

de Lima Batista, Anderson Márcio; Miranda, Marcus Aurélio Ribeiro; Martins, Fátima Itana Chaves Custódio

Several methods can be used to obtain, from powder diffraction patterns, crystallite size and lattice strain of polycrystalline samples. Some examples are the Scherrer equation, Williamson–Hall plots, Warren/Averbach Fourier decomposition, Whole Powder Pattern Modeling, and Debye function analysis. To apply some of these methods, it is necessary to remove the contribution of the instrument to the widths of the diffraction peaks. Nowadays, one of the main samples used for this purpose is the LaB6 SRM660b commercialized by the National Institute of Standard Technology; the width of the diffraction peak of this sample is caused only by the instrumental apparatus. However,more » this sample can be expensive for researchers in developing countries. In this work, the authors present a simple route to obtain micron-sized polycrystalline CeO 2that have a full width at half maximum comparable with the SRM660b and therefore it can be used to remove instrumental broadening.« less

Three-energy focusing Laue monochromator for the diamond light source x-ray pair distribution function beamline I15-1

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

Sutter, John P., E-mail: john.sutter@diamond.ac.uk; Chater, Philip A.; Hillman, Michael R.

2016-07-27

The I15-1 beamline, the new side station to I15 at the Diamond Light Source, will be dedicated to the collection of atomic pair distribution function data. A Laue monochromator will be used consisting of three silicon crystals diffracting X-rays at a common Bragg angle of 2.83°. The crystals use the (1 1 1), (2 2 0), and (3 1 1) planes to select 40, 65, and 76 keV X-rays, respectively, and will be bent meridionally to horizontally focus the selected X-rays onto the sample. All crystals will be cut to the same optimized asymmetry angle in order to eliminate imagemore » broadening from the crystal thickness. Finite element calculations show that the thermal distortion of the crystals will affect the image size and bandpass.« less

Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II

DOE PAGES

Nazaretski, E.; Yan, H.; Lauer, K.; ...

2017-10-05

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ~15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature ofmore » a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.« less

Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II

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

Nazaretski, E.; Yan, H.; Lauer, K.

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ~15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature ofmore » a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.« less

Addressing the amorphous content issue in quantitative phase analysis : the certification of NIST SRM 676a.

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

Cline, J. P.; Von Dreele, R. B.; Winburn, R.

2011-07-01

A non-diffracting surface layer exists at any boundary of a crystal and can comprise a mass fraction of several percent in a finely divided solid. This has led to the long-standing issue of amorphous content in standards for quantitative phase analysis (QPA). NIST standard reference material (SRM) 676a is a corundum ({alpha}-Al{sub 2}O{sub 3}) powder, certified with respect to phase purity for use as an internal standard in powder diffraction QPA. The amorphous content of SRM 676a is determined by comparing diffraction data from mixtures with samples of silicon powders that were engineered to vary their specific surface area. Undermore » the (supported) assumption that the thickness of an amorphous surface layer on Si was invariant, this provided a method to control the crystalline/amorphous ratio of the silicon components of 50/50 weight mixtures of SRM 676a with silicon. Powder diffraction experiments utilizing neutron time-of-flight and 25 keV and 67 keV X-ray energies quantified the crystalline phase fractions from a series of specimens. Results from Rietveld analyses, which included a model for extinction effects in the silicon, of these data were extrapolated to the limit of zero amorphous content of the Si powder. The certified phase purity of SRM 676a is 99.02% {+-} 1.11% (95% confidence interval). This novel certification method permits quantification of amorphous content for any sample of interest, by spiking with SRM 676a.« less

Addressing the Amorphous Content Issue in Quantitative Phase Analysis: The Certification of NIST Standard Reference Material 676a

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

J Cline; R Von Dreele; R Winburn

2011-12-31

A non-diffracting surface layer exists at any boundary of a crystal and can comprise a mass fraction of several percent in a finely divided solid. This has led to the long-standing issue of amorphous content in standards for quantitative phase analysis (QPA). NIST standard reference material (SRM) 676a is a corundum ({alpha}-Al{sub 2}O{sub 3}) powder, certified with respect to phase purity for use as an internal standard in powder diffraction QPA. The amorphous content of SRM 676a is determined by comparing diffraction data from mixtures with samples of silicon powders that were engineered to vary their specific surface area. Undermore » the (supported) assumption that the thickness of an amorphous surface layer on Si was invariant, this provided a method to control the crystalline/amorphous ratio of the silicon components of 50/50 weight mixtures of SRM 676a with silicon. Powder diffraction experiments utilizing neutron time-of-flight and 25 keV and 67 keV X-ray energies quantified the crystalline phase fractions from a series of specimens. Results from Rietveld analyses, which included a model for extinction effects in the silicon, of these data were extrapolated to the limit of zero amorphous content of the Si powder. The certified phase purity of SRM 676a is 99.02% {+-} 1.11% (95% confidence interval). This novel certification method permits quantification of amorphous content for any sample of interest, by spiking with SRM 676a.« less

Instrumentation For Diffraction Enhanced Imaging Experiments At HASYLAB

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

Lohmann, M.; Dix, W.-R.; Metge, J.

The new X-ray radiography imaging technique, named diffraction enhanced imaging (DEI), enables almost scatter free absorption imaging, the production of the so-called refraction images of a sample. The images show improved contrast compared to standard imaging applications. At the HASYLAB wiggler beamline W2 at the 2nd-generation storage ring DORIS a 5cm wide beam with an adjustable energy between 10 and 70keV is available. A Si [111] pre-monochromator is used followed by the main monochromator using the (111) or the (333)-reflection. Visualization of fossils, detecting internal pearl structures, monitoring of bone and cartilage and documentation of implant healing in bone aremore » application examples at HASYLAB.« less

High pressure single-crystal micro X-ray diffraction analysis with GSE_ADA/RSV software

NASA Astrophysics Data System (ADS)

Dera, Przemyslaw; Zhuravlev, Kirill; Prakapenka, Vitali; Rivers, Mark L.; Finkelstein, Gregory J.; Grubor-Urosevic, Ognjen; Tschauner, Oliver; Clark, Simon M.; Downs, Robert T.

2013-08-01

GSE_ADA/RSV is a free software package for custom analysis of single-crystal micro X-ray diffraction (SCμXRD) data, developed with particular emphasis on data from samples enclosed in diamond anvil cells and subject to high pressure conditions. The package has been in extensive use at the high pressure beamlines of Advanced Photon Source (APS), Argonne National Laboratory and Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. The software is optimized for processing of wide-rotation images and includes a variety of peak intensity corrections and peak filtering features, which are custom-designed to make processing of high pressure SCμXRD easier and more reliable.

Crystallographic Phasing from Weak Anomalous Signals

PubMed Central

Liu, Qun; Hendrickson, Wayne A.

2015-01-01

The exploitation of anomalous signals for biological structural solution is maturing. Single-wavelength anomalous diffraction (SAD) is dominant in de novo structure analysis. Nevertheless, for challenging structures where the resolution is low (dmin ≥ 3.5 Å) or where only lighter atoms (Z ≤ 20) are present, as for native macromolecules, solved SAD structures are still scarce. With the recent rapid development in crystal handling, beamline instrumentation, optimization of data collection strategies, use of multiple crystals and structure determination technologies, the weak anomalous diffraction signals are now robustly measured and should be used for routine SAD structure determination. The review covers these recent advances on weak anomalous signals measurement, analysis and utilization. PMID:26432413

Crystallographic phasing from weak anomalous signals.

PubMed

Liu, Qun; Hendrickson, Wayne A

2015-10-01

The exploitation of anomalous signals for biological structural solution is maturing. Single-wavelength anomalous diffraction (SAD) is dominant in de novo structure analysis. Nevertheless, for challenging structures where the resolution is low (dmin≥3.5Å) or where only lighter atoms (Z≤20) are present, as for native macromolecules, solved SAD structures are still scarce. With the recent rapid development in crystal handling, beamline instrumentation, optimization of data collection strategies, use of multiple crystals and structure determination technologies, the weak anomalous diffraction signals are now robustly measured and should be used for routine SAD structure determination. The review covers these recent advances on weak anomalous signals measurement, analysis and utilization. Copyright © 2015 Elsevier Ltd. All rights reserved.

Additional evidence from x-ray powder diffraction patterns that icosahedral quasi-crystals of intermetallic compounds are twinned cubic crystals

PubMed Central

Pauling, Linus

1988-01-01

Analysis of the measured values of Q for the weak peaks (small maxima, usually considered to be background fluctuations, “noise”) on the x-ray powder diffraction curves for 17 rapidly quenched alloys leads directly to the conclusion that they are formed by an 820-atom or 1012-atom primitive cubic structure that by icosahedral twinning produces the so-called icosahedral quasi-crystals. PMID:16593948

Test and Delivery of the Chemin Mineralogical Instrument for Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Blake, D. F.; Vaniman, D.; Anderson, R.; Bish, D.; Chipera, S.; Chemtob, S.; Crisp, J.; DesMarais, D. J.; Downs, R.; Feldman, S.;

Melting point suppression in new lanthanoid(III) ionic liquids by trapping of kinetic polymorphs: an in situ synchrotron powder diffraction study.

PubMed

Chesman, Anthony S R; Yang, Mei; Mallick, Bert; Ross, Tamsyn M; Gass, Ian A; Deacon, Glen B; Batten, Stuart R; Mudring, Anja-Verena

2012-01-04

The complexes (N(4444))(3)[Ln(dcnm)(6)] (Ln = La-Nd, Sm; N(4444) = tetrabutylammonium) display a decrease in the melting point upon fast cooling from a melt, which is shown by in situ synchrotron based X-ray powder diffraction to be due to the formation of a second, less thermodynamically stable, polymorph. This journal is © The Royal Society of Chemistry 2012

Clifford G. Shull, Neutron Diffraction, Hydrogen Atoms, and Neutron

Science.gov Websites

Analysis of NaH and NaD, DOE Technical Report, April 1947 The Diffraction of Neutrons by Crystalline Powders; DOE Technical Report; 1948 Neutron Diffraction Studies, DOE Technical Report, 1948 Laue Structure of Thorium and Zirconium Dihydrides by X-ray and Neutron Diffraction, DOE Technical Report, April

Effect of powder compaction on radiation-thermal synthesis of lithium-titanium ferrites

NASA Astrophysics Data System (ADS)

Surzhikov, A. P.; Lysenko, E. N.; Vlasov, V. A.; Malyshev, A. V.; Korobeynikov, M. V.; Mikhailenko, M. A.

2017-01-01

Effect of powder compaction on the efficiency of thermal and radiation-thermal synthesis of lithium-substituted ferrites was investigated by X-Ray diffraction and specific magnetization analysis. It was shown that the radiation-thermal heating of compacted powder reagents mixture leads to an increase in efficiency of lithium-titanium ferrites synthesis.

Synthesis of nano-forsterite powder by making use of natural silica sand

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

Nurbaiti, Upik, E-mail: upik-nurbaiti@mail.unnes.ac.id; Department of Physics, Faculty of Mathematics and Natural Sciences Semarang State University Jl. Raya Sekaran GunungPati, Semarang 50221; Suud, Fikriyatul Azizah

2016-02-08

Nano-forsterite powder with natural silica sand and magnesium powder as the raw materials have been succesfully synthesized. The silica sand was purified followed by a coprecipitation process to obtain colloidal silica. The magnesium powder was dissolved in a chloric acid solution to obtain MgCl{sub 2} solution. The nanoforsterite powder was synthesised using a sol-gel method which included the mixing the colloidal silica and the MgCl{sub 2} solution with various aging and filtering processes. The samples were dried at 100 °C using a hot plate and then the dried powders were calcinated at 900 °C for 2 hours. The samples weremore » characetised for their elements and phase compositions using X-ray Flourescence (XRF) and X-ray Diffraction (XRD) methods, respectively. The diffraction data were qualitatively analyzed using Match!2 software and quantitatively using Rietica software. The crystallite size was verified using Transmission Electron Microscopy (TEM). Results of XRD data analysis showed that the forsterite content reached up to 90.5% wt. The TEM average crystallite size was approximately 53(6) nm.« less

Crystal structure of methylprednisolone acetate form II, C 24H 32O 6

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

Wheatley, Austin M.; Kaduk, James A.; Gindhart, Amy M.

The crystal structure of methylprednisolone acetate form II, C 24H 32O 6, has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Methylprednisolone acetate crystallizes in space groupP2 12 12 1(#19) witha= 8.17608(2),b= 9.67944(3),c= 26.35176(6) Å,V= 2085.474(6) Å 3, andZ= 4. Both hydroxyl groups act as hydrogen bond donors, resulting in a two-dimensional hydrogen bond network in theabplane. C–H…O hydrogen bonds also contribute to the crystal energy. The powder pattern is included in the Powder Diffraction File™ as entry 00-065-1412.

Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments

NASA Astrophysics Data System (ADS)

Schlicker, Lukas; Doran, Andrew; Schneppmüller, Peter; Gili, Albert; Czasny, Mathias; Penner, Simon; Gurlo, Aleksander

2018-03-01

This work describes a device for time-resolved synchrotron-based in situ and operando X-ray powder diffraction measurements at elevated temperatures under controllable gaseous environments. The respective gaseous sample environment is realized via a gas-tight capillary-in-capillary design, where the gas flow is achieved through an open-end 0.5 mm capillary located inside a 0.7 mm capillary filled with a sample powder. Thermal mass flow controllers provide appropriate gas flows and computer-controlled on-the-fly gas mixing capabilities. The capillary system is centered inside an infrared heated, proportional integral differential-controlled capillary furnace allowing access to temperatures up to 1000 °C.

Microcrystallography using single-bounce monocapillary optics

PubMed Central

Gillilan, R. E.; Cook, M. J.; Cornaby, S. W.; Bilderback, D. H.

2010-01-01

X-ray microbeams have become increasingly valuable in protein crystallography. A number of synchrotron beamlines worldwide have adapted to handling smaller and more challenging samples by providing a combination of high-precision sample-positioning hardware, special visible-light optics for sample visualization, and small-diameter X-ray beams with low background scatter. Most commonly, X-ray microbeams with diameters ranging from 50 µm to 1 µm are produced by Kirkpatrick and Baez mirrors in combination with defining apertures and scatter guards. A simple alternative based on single-bounce glass monocapillary X-ray optics is presented. The basic capillary design considerations are discussed and a practical and robust implementation that capitalizes on existing beamline hardware is presented. A design for mounting the capillary is presented which eliminates parasitic scattering and reduces deformations of the optic to a degree suitable for use on next-generation X-ray sources. Comparison of diffraction data statistics for microcrystals using microbeam and conventional aperture-collimated beam shows that capillary-focused beam can deliver significant improvement. Statistics also confirm that the annular beam profile produced by the capillary optic does not impact data quality in an observable way. Examples are given of new structures recently solved using this technology. Single-bounce monocapillary optics can offer an attractive alternative for retrofitting existing beamlines for microcrystallography. PMID:20157276

Effects of Peripheral Architecture on the Properties of Aryl Polyhedral Oligomeric Silsesquioxanes

DTIC Science & Technology

2012-07-26

POSS) molecules are described. These POSS materials were synthesized in our laboratory and characterized by single-crystal and powder X - ray diffraction ...powder X - ray diffraction (XRD), where applicable. 1H, 13C, and 29Si NMR spectra were obtained on Bruker 300 and 400 MHz spectrometers using 5 mm o.d...degree of cage ordering during precipitation. Referring back to Figure 14, strong X - ray scattering peaks in the spectra for 1 in the d- spacing range

Insertion of Guest Molecules into a Mixed Ligand Metal-Organic Framework via Single-Crystal-to-Single Crystal Guest Exchange

DTIC Science & Technology

2014-07-01

powder x-ray diffraction (PXRD), thermogravimentric analysis (TGA), and Fourier transform infrared (FTIR). 15. SUBJECT TERMS Metal organic frame work...the inclusion by using a variety of analytical techniques, such as powder x-ray diffraction (PXRD), thermo-gravimetric analysis (TGA), Fourier...Characterizations Analysis of the MOF and the complexes with the MOF and the guest molecules was performed using an Agilent GC-MS (Model 6890N GC and Model 5973N

Testing the limits of sensitivity in a solid-state structural investigation by combined X-ray powder diffraction, solid-state NMR, and molecular modelling.

PubMed

Filip, Xenia; Borodi, Gheorghe; Filip, Claudiu

2011-10-28

A solid state structural investigation of ethoxzolamide is performed on microcrystalline powder by using a multi-technique approach that combines X-ray powder diffraction (XRPD) data analysis based on direct space methods with information from (13)C((15)N) solid-state Nuclear Magnetic Resonance (SS-NMR) and molecular modeling. Quantum chemical computations of the crystal were employed for geometry optimization and chemical shift calculations based on the Gauge Including Projector Augmented-Wave (GIPAW) method, whereas a systematic search in the conformational space was performed on the isolated molecule using a molecular mechanics (MM) approach. The applied methodology proved useful for: (i) removing ambiguities in the XRPD crystal structure determination process and further refining the derived structure solutions, and (ii) getting important insights into the relationship between the complex network of non-covalent interactions and the induced supra-molecular architectures/crystal packing patterns. It was found that ethoxzolamide provides an ideal case study for testing the accuracy with which this methodology allows to distinguish between various structural features emerging from the analysis of the powder diffraction data. This journal is © the Owner Societies 2011

Hard X-ray polarizer to enable simultaneous three-dimensional nanoscale imaging of magnetic structure and lattice strain

DOE PAGES

Logan, Jonathan; Harder, Ross; Li, Luxi; ...

2016-01-01

Recent progress in the development of dichroic Bragg coherent diffractive imaging, a new technique for simultaneous three-dimensional imaging of strain and magnetization at the nanoscale, is reported. This progress includes the installation of a diamond X-ray phase retarder at beamline 34-ID-C of the Advanced Photon Source. Here, the performance of the phase retarder for tuning X-ray polarization is demonstrated with temperature-dependent X-ray magnetic circular dichroism measurements on a gadolinium foil in transmission and on a Gd 5Si 2Ge 2crystal in diffraction geometry with a partially coherent, focused X-ray beam. Feasibility tests for dichroic Bragg coherent diffractive imaging are presented. Thesemore » tests include (1) using conventional Bragg coherent diffractive imaging to determine whether the phase retarder introduces aberrations using a nonmagnetic gold nanocrystal as a control sample, and (2) collecting coherent diffraction patterns of a magnetic Gd 5Si 2Ge 2nanocrystal with left- and right-circularly polarized X-rays. Future applications of dichroic Bragg coherent diffractive imaging for the correlation of strain and lattice defects with magnetic ordering and inhomogeneities are considered.« less

Composition and particle size of electrolytic copper powders prepared in water-containing dimethyl sulfoxide electrolytes

NASA Astrophysics Data System (ADS)

Mamyrbekova, Aigul'; Abzhalov, B. S.; Mamyrbekova, Aizhan

2017-07-01

The possibility of the electroprecipitation of copper powder via the cathodic reduction of an electrolyte solution containing copper(II) nitrate trihydrate and dimethyl sulfoxide (DMSO) is shown. The effect electrolysis conditions (current density, concentration and temperature of electrolyte) have on the dimensional characteristics of copper powder is studied. The size and shape of the particles of the powders were determined by means of electron microscopy; the qualitative composition of the powders, with X-ray diffraction.

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials.

PubMed

Kulriya, P K; Singh, F; Tripathi, A; Ahuja, R; Kothari, A; Dutt, R N; Mishra, Y K; Kumar, Amit; Avasthi, D K

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

Coherent soft X-ray diffraction imaging of coliphage PR772 at the Linac coherent light source

PubMed Central

Reddy, Hemanth K.N.; Yoon, Chun Hong; Aquila, Andrew; Awel, Salah; Ayyer, Kartik; Barty, Anton; Berntsen, Peter; Bielecki, Johan; Bobkov, Sergey; Bucher, Maximilian; Carini, Gabriella A.; Carron, Sebastian; Chapman, Henry; Daurer, Benedikt; DeMirci, Hasan; Ekeberg, Tomas; Fromme, Petra; Hajdu, Janos; Hanke, Max Felix; Hart, Philip; Hogue, Brenda G.; Hosseinizadeh, Ahmad; Kim, Yoonhee; Kirian, Richard A.; Kurta, Ruslan P.; Larsson, Daniel S.D.; Duane Loh, N.; Maia, Filipe R.N.C.; Mancuso, Adrian P.; Mühlig, Kerstin; Munke, Anna; Nam, Daewoong; Nettelblad, Carl; Ourmazd, Abbas; Rose, Max; Schwander, Peter; Seibert, Marvin; Sellberg, Jonas A.; Song, Changyong; Spence, John C.H.; Svenda, Martin; Van der Schot, Gijs; Vartanyants, Ivan A.; Williams, Garth J.; Xavier, P. Lourdu

2017-01-01

Single-particle diffraction from X-ray Free Electron Lasers offers the potential for molecular structure determination without the need for crystallization. In an effort to further develop the technique, we present a dataset of coherent soft X-ray diffraction images of Coliphage PR772 virus, collected at the Atomic Molecular Optics (AMO) beamline with pnCCD detectors in the LAMP instrument at the Linac Coherent Light Source. The diameter of PR772 ranges from 65–70 nm, which is considerably smaller than the previously reported ~600 nm diameter Mimivirus. This reflects continued progress in XFEL-based single-particle imaging towards the single molecular imaging regime. The data set contains significantly more single particle hits than collected in previous experiments, enabling the development of improved statistical analysis, reconstruction algorithms, and quantitative metrics to determine resolution and self-consistency. PMID:28654088

Coherent soft X-ray diffraction imaging of coliphage PR772 at the Linac coherent light source

DOE PAGES

Reddy, Hemanth K. N.; Yoon, Chun Hong; Aquila, Andrew; ...

2017-06-27

Single-particle diffraction from X-ray Free Electron Lasers offers the potential for molecular structure determination without the need for crystallization. In an effort to further develop the technique, we present a dataset of coherent soft X-ray diffraction images of Coliphage PR772 virus, collected at the Atomic Molecular Optics (AMO) beamline with pnCCD detectors in the LAMP instrument at the Linac Coherent Light Source. The diameter of PR772 ranges from 65–70 nm, which is considerably smaller than the previously reported ~600 nm diameter Mimivirus. This reflects continued progress in XFEL-based single-particle imaging towards the single molecular imaging regime. As a result, themore » data set contains significantly more single particle hits than collected in previous experiments, enabling the development of improved statistical analysis, reconstruction algorithms, and quantitative metrics to determine resolution and self-consistency.« less

In-situ data collection at the photon factory macromolecular crystallography beamlines

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

Yamada, Yusuke, E-mail: yusuke.yamada@kek.jp; Matsugaki, Naohiro; Kato, Ryuichi

Crystallization trial is one of the most important but time-consuming steps in macromolecular crystallography, and in-situ diffraction experiment has a capability to make researchers to proceed this step more efficiently. At the Photon Factory, a new tabletop diffractometer for in-situ diffraction experiments has been developed. It consists of XYZ translation stages with a plate handler, an on-axis viewing system and a plate rack with a capacity for ten crystallization plates. These components sit on a common plate and are able to be placed on the existing diffractometer table. The CCD detector with a large active area and a pixel arraymore » detector with a small active area are used for acquiring diffraction images from crystals. Dedicated control software and a user interface have also been developed. The new diffractometer has been operational for users and used for evaluation of crystallization screening since 2014.« less

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

NASA Astrophysics Data System (ADS)

Kulriya, P. K.; Singh, F.; Tripathi, A.; Ahuja, R.; Kothari, A.; Dutt, R. N.; Mishra, Y. K.; Kumar, Amit; Avasthi, D. K.

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T =255K.

Coherent soft X-ray diffraction imaging of coliphage PR772 at the Linac coherent light source.

PubMed

Reddy, Hemanth K N; Yoon, Chun Hong; Aquila, Andrew; Awel, Salah; Ayyer, Kartik; Barty, Anton; Berntsen, Peter; Bielecki, Johan; Bobkov, Sergey; Bucher, Maximilian; Carini, Gabriella A; Carron, Sebastian; Chapman, Henry; Daurer, Benedikt; DeMirci, Hasan; Ekeberg, Tomas; Fromme, Petra; Hajdu, Janos; Hanke, Max Felix; Hart, Philip; Hogue, Brenda G; Hosseinizadeh, Ahmad; Kim, Yoonhee; Kirian, Richard A; Kurta, Ruslan P; Larsson, Daniel S D; Duane Loh, N; Maia, Filipe R N C; Mancuso, Adrian P; Mühlig, Kerstin; Munke, Anna; Nam, Daewoong; Nettelblad, Carl; Ourmazd, Abbas; Rose, Max; Schwander, Peter; Seibert, Marvin; Sellberg, Jonas A; Song, Changyong; Spence, John C H; Svenda, Martin; Van der Schot, Gijs; Vartanyants, Ivan A; Williams, Garth J; Xavier, P Lourdu

2017-06-27

Single-particle diffraction from X-ray Free Electron Lasers offers the potential for molecular structure determination without the need for crystallization. In an effort to further develop the technique, we present a dataset of coherent soft X-ray diffraction images of Coliphage PR772 virus, collected at the Atomic Molecular Optics (AMO) beamline with pnCCD detectors in the LAMP instrument at the Linac Coherent Light Source. The diameter of PR772 ranges from 65-70 nm, which is considerably smaller than the previously reported ~600 nm diameter Mimivirus. This reflects continued progress in XFEL-based single-particle imaging towards the single molecular imaging regime. The data set contains significantly more single particle hits than collected in previous experiments, enabling the development of improved statistical analysis, reconstruction algorithms, and quantitative metrics to determine resolution and self-consistency.

Crystallographic Determination of Molecular Parameters for K2SiF6: A Physical Chemistry Laboratory Experiment.

ERIC Educational Resources Information Center

Loehlin, James H.; Norton, Alexandra P.

1988-01-01

Describes a crystallography experiment using both diffraction-angle and diffraction-intensity information to determine the lattice constant and a lattice independent molecular parameter, while still employing standard X-ray powder diffraction techniques. Details the method, experimental details, and analysis for this activity. (CW)

Structural, microstructural and magnetic evolution in cryo milled carbon doped MnAl.

PubMed

Fang, Hailiang; Cedervall, Johan; Hedlund, Daniel; Shafeie, Samrand; Deledda, Stefano; Olsson, Fredrik; von Fieandt, Linus; Bednarcik, Jozef; Svedlindh, Peter; Gunnarsson, Klas; Sahlberg, Martin

2018-02-06

The low cost, rare earth free τ-phase of MnAl has high potential to partially replace bonded Nd 2 Fe 14 B rare earth permanent magnets. However, the τ-phase is metastable and it is experimentally difficult to obtain powders suitable for the permanent magnet alignment process, which requires the fine powders to have an appropriate microstructure and high τ-phase purity. In this work, a new method to make high purity τ-phase fine powders is presented. A high purity τ-phase Mn 0.55 Al 0.45 C 0.02 alloy was synthesized by the drop synthesis method. The drop synthesized material was subjected to cryo milling and  followed by a flash heating process. The crystal structure and microstructure of the drop synthesized, cryo milled and flash heated samples were studied by X-ray in situ powder diffraction, scanning electron microscopy, X-ray energy dispersive spectroscopy and electron backscatter diffraction. Magnetic properties and magnetic structure of the drop synthesized, cryo milled, flash heated  samples were characterized by magnetometry and neutron powder diffraction, respectively. The results reveal that the 2 and 4 hours cryo milled and flash heated samples both exhibit high τ-phase purity and micron-sized round particle shapes. Moreover, the flash heated samples display high saturation magnetization as well as increased coercivity.

Phase diagram of the relaxor ferroelectric (1- x )Pb(Mg 1/3Nb 2/3)O 3+ x PbTiO 3 revisited: a neutron powder diffraction study of the relaxor skin effect

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

Phelan, D.; Rodriguez, E. E.; Gao, J.

2014-11-17

We revisit the phase diagram of the relaxor ferroelectric PMN- xPT using neutron powder diffraction to test suggestions that residual oxygen vacancies and/or strain affect the ground state crystal structure. Powdered samples of PMN- xPT were prepared with nominal compositions of x = 0:10, 0.20, 0.30, and 0.40 and divided into two identical sets, one of which was annealed in air to relieve grinding-induced strain and to promote an ideal oxygen stoichiometry. For a given composition and temperature the same structural phase is observed for each specimen. However, the distortions in all of the annealed samples are smaller than thosemore » in the as-grown samples. Further, the diffraction patterns for x = 0:10, 0.20, and 0.30 are best refined using the monoclinic Cm space group. By comparing our neutron diffraction results to those obtained on single crystals having similar compositions, we conclude that the relaxor skin effect in PMN- xPT vanishes on the Ti-rich side of the morphotropic phase boundary.« less

POWTEX Neutron Diffractometer at FRM II - New Perspectives in Rock Deformation and Recrystallisation Analysis

NASA Astrophysics Data System (ADS)

Walter, J. M.; Stipp, M.; Ullemeyer, K.; Klein, H.; Leiss, B.; Hansen, B.; Kuhs, W. F.

2011-12-01

Neutron diffraction has become a routine method in Geoscience for the quantitative analysis of crystallographic preferred orientations (CPOs) and for (experimental) powder diffraction. Quantitative texture analysis is a common tool for the investigation of fabric development in mono- and polyphase rocks, their deformation histories and kinematics. Furthermore the quantitative characterization of anisotropic physical properties by bulk texture measurements can be achieved due to the high penetration capabilities of neutrons. To cope with increasing needs for beam time at neutron diffraction facilities with the corresponding technical characteristics and equipment, POWTEX (POWder and TEXture Diffractometer) is designed as a high-intensity diffractometer at the neutron research reactor FRM II in Garching, Germany by groups from the RWTH Aachen, Forschungszentrum Jülich and the University of Göttingen. Complementary to existing neutron diffractometers (SKAT at Dubna, Russia; GEM at ISIS, UK; HIPPO at Los Alamos, USA; D20 at ILL, France; and the local STRESS-SPEC and SPODI at FRM II) the layout of POWTEX is focused on fast (texture) measurements for either time-resolved experiments or the measurement of larger sample series as necessary for the study of large scale geological structures. By utilizing a range of neutron wavelengths simultaneously (TOF-technique), a high flux (~1 x 107 n/cm2s) and a high detector coverage ( 9.8 sr) effective texture measurements without sample tilting and rotation are possible. Furthermore the instrument and the angular detector resolution is sufficient for strong recrystallisation textures as well as weak textures of polyphase rocks. Thereby large sample environments will be implemented at POWTEX allowing in-situ time-resolved texture measurements during deformation experiments on rocksalt, ice and other materials. Furthermore a furnace for 3D-recrystallisation analysis of single grains will be realized complementary to the furnace that already exists for fine grained materials at the synchrotron beamline BW5 at HASYLAB, Germany (e.g. Klein et al. 2009). The in-situ triaxial deformation apparatus is operated by a uniaxial spindle drive with a maximum axial load of 200 kN, which will be redesigned to minimize shadowing effects on the detector. The HT experiments will be carried out in uniaxial compression or extension and an upgrade to triaxial deformation conditions is envisaged. The load frame can alternatively be used for ice deformation by inserting a cryostat cell for temperatures down to 77 K with a triaxial apparatus allowing also simple shear experiments on ice. Strain rates range between 10-8 and 10-3 s-1 reaching to at least 50 % axial strain. The furnace for the recrystallization analysis will be a mirror furnace with temperatures up to 1500° C, which will be rotatable around a vertical axis to obtain the required stereologic orientation information.

Hydrogenation properties of Li{sub x}Sr{sub 1−x}AlSi studied by quantum-chemical methods (0≤x≤1) and in-situ neutron powder diffraction (x=1)

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

Kunkel, Nathalie, E-mail: nathalie.kunkel@chimie-paristech.fr; FR 8.1 Universität des Saarlandes, Postach 151150, 66041 Saarbrücken; Reichert, Christian

2015-01-15

In-situ neutron powder diffraction studies of the Half-Heusler phase LiAlSi under high deuterium pressures and first principle calculations of solid solutions of Li{sub x}Sr{sub 1−x}AlSi and their hydrides Li{sub x}Sr{sub 1−x}AlSiH were carried out. In contrast to an earlier study, there is no experimental evidence for hydrogen (deuterium) uptake up to gas pressures of 15 MPa and temperatures of 550 °C. Instead a slow decomposition reaction according to LiAlSi+1/2H{sub 2}=LiH+Al+Si was found by in-situ neutron powder diffraction. Theoretical calculations by DFT methods on hypothetical solid solutions of Li{sub x}Sr{sub 1−x}AlSi show the LiAlSi type to be the energetically most stablemore » structure for 0.7« less

The Macromolecular Neutron Diffractometer MaNDi at the Spallation Neutron Source

DOE PAGES

Coates, Leighton; Cuneo, Matthew J.; Frost, Matthew J.; ...

2015-07-18

The Macromolecular Neutron Diffractometer (MaNDi) is located on beamline 11B of the Spallation Neutron Source at Oak Ridge National Laboratory. Moreover, the instrument is a neutron time-of-flight wavelength-resolved Laue diffractometer optimized to collect diffraction data from single crystals. Finally, the instrument has been designed to provide flexibility in several instrumental parameters, such as beam divergence and wavelength bandwidth, to allow data collection from a range of macromolecular systems.

Sub-500  nm hard x ray focusing by compound long kinoform lenses.

PubMed

Liao, Keliang; Liu, Jing; Liang, Hao; Wu, Xuehui; Zhang, Kai; Yuan, Qingxi; Yi, Futing; Sheng, Weifan

2016-01-01

The focusing performance of polymethyl methacrylate compound long kinoform lenses with 70 μm aperture and 19.5 mm focal length was characterized with 8 keV x rays using the knife-edge scan method at the 4W1A transmission x-ray microscope beamline of Beijing Synchrotron Radiation Facility. The experiment result shows a best FWHM focus size of 440 nm with 31% diffraction efficiency.

Diffraction gratings metrology and ray-tracing results for an XUV Raman spectrometer at FLASH

PubMed Central

Dziarzhytski, Siarhei; Siewert, Frank; Gwalt, Grzegorz; Seliger, Tino; Rübhausen, Michael; Weigelt, Holger; Brenner, Günter

2018-01-01

The extreme-ultraviolet double-stage imaging Raman spectrometer is a permanent experimental endstation at the plane-grating monochromator beamline branch PG1 at FLASH at DESY in Hamburg, Germany. This unique instrument covers the photon energy range from 20 to 200 eV with high energy resolution of about 2 to 20 meV (design values) featuring an efficient elastic line suppression as well as effective stray light rejection. Such a design enables studies of low-energy excitations like, for example, phonons in solids close to the vicinity of the elastic line. The Raman spectrometer effectively operates with four reflective off-axial parabolic mirrors and two plane-grating units. The optics quality and their precise alignment are crucial to guarantee best performance of the instrument. Here, results on a comprehensive investigation of the quality of the spectrometer diffraction gratings are presented. The gratings have been characterized by ex situ metrology at the BESSY-II Optics Laboratory, employing slope measuring deflectometry and interferometry as well as atomic force microscopy studies. The efficiency of these key optical elements has been measured at the at-wavelength metrology laboratory using the reflectometer at the BESSY-II Optics beamline. Also, the metrology results are discussed with respect to the expected resolving power of the instrument by including them in ray-tracing studies of the instrument. PMID:29271763

An experimental apparatus for diffraction-limited soft x-ray nano-focusing

NASA Astrophysics Data System (ADS)

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

2011-09-01

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. Visible-light long-trace profilometry was used to pre-align the mirror before installation at the beamline. 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.

Instrumental development of a quasi-relativistic ultrashort electron beam source for electron diffractions and spectroscopies

NASA Astrophysics Data System (ADS)

Shin, Young-Min; Figora, Michael

2017-10-01

A stable femtosecond electron beam system has been configured for time-resolved pump-probe experiments. The ultrafast electron diffraction (UED) system is designed with a sub-MeV photoelectron beam source pulsed by a femtosecond UV laser and nondispersive beamline components, including a bunch compressor—a pulsed S-band klystron is installed and fully commissioned with 5.5 MW peak power in a 2.5 μs pulse length. A single-cell RF photo-gun is designed to produce 1.6-16 pC electron bunches in a photoemission mode with 150 fs pulse duration at 0.5-1 MeV. The measured RF system jitters are within 1% in magnitude and 0.2° in phase, which would induce 3.4 keV and 0.25 keV of ΔE, corresponding to 80 fs and 5 fs of Δt, respectively. Our particle-in-cell simulations indicate that the designed bunch compressor reduces the time-of-arrival jitter by about an order of magnitude. The transport and focusing optics of the designed beamline with the bunch compressor enables an energy spread within 10-4 and a bunch length (electron probe) within <500 fs. In this paper, the design analysis and instrumental test results are presented along with the development of the quasi-relativistic UED system.

Instrumental development of a quasi-relativistic ultrashort electron beam source for electron diffractions and spectroscopies.

PubMed

Shin, Young-Min; Figora, Michael

2017-10-01

A stable femtosecond electron beam system has been configured for time-resolved pump-probe experiments. The ultrafast electron diffraction (UED) system is designed with a sub-MeV photoelectron beam source pulsed by a femtosecond UV laser and nondispersive beamline components, including a bunch compressor-a pulsed S-band klystron is installed and fully commissioned with 5.5 MW peak power in a 2.5 μs pulse length. A single-cell RF photo-gun is designed to produce 1.6-16 pC electron bunches in a photoemission mode with 150 fs pulse duration at 0.5-1 MeV. The measured RF system jitters are within 1% in magnitude and 0.2° in phase, which would induce 3.4 keV and 0.25 keV of ΔE, corresponding to 80 fs and 5 fs of Δt, respectively. Our particle-in-cell simulations indicate that the designed bunch compressor reduces the time-of-arrival jitter by about an order of magnitude. The transport and focusing optics of the designed beamline with the bunch compressor enables an energy spread within 10 -4 and a bunch length (electron probe) within <500 fs. In this paper, the design analysis and instrumental test results are presented along with the development of the quasi-relativistic UED system.

Amorphous and liquid samples structure and density measurements at high pressure - high temperature using diffraction and imaging techniques

NASA Astrophysics Data System (ADS)

Guignot, N.; King, A.; Clark, A. N.; Perrillat, J. P.; Boulard, E.; Morard, G.; Deslandes, J. P.; Itié, J. P.; Ritter, X.; Sanchez-Valle, C.

2016-12-01

Determination of the density and structure of liquids such as iron alloys, silicates and carbonates is a key to understand deep Earth structure and dynamics. X-ray diffraction provided by large synchrotron facilities gives excellent results as long as the signal scattered from the sample can be isolated from its environment. Different techniques already exist; we present here the implementation and the first results given by the combined angle- and energy-dispersive structural analysis and refinement (CAESAR) technique introduced by Wang et al. in 2004, that has never been used in this context. It has several advantages in the study of liquids: 1/ the standard energy-dispersive technique (EDX), fast and compatible with large multi-anvil presses frames, is used for fast analysis free of signal pollution from the sample environment 2/ some limitations of the EDX technique (homogeneity of the sample, low resolution) are irrelevant in the case of liquid signals, others (wrong intensities, escape peaks artifacts, background subtraction) are solved by the CAESAR technique 3/ high Q data (up to 15 A-1 and more) can be obtained in a few hours (usually less than 2). We present here the facilities available on the PSICHE beamline (SOLEIL synchrotron, France) and a few results obtained using a Paris-Edinburgh (PE) press and a 1200 tons load capacity multi-anvil press with a (100) DIA compression module. X-ray microtomography, used in conjunction with a PE press featuring rotating anvils (RotoPEc, Philippe et al., 2013) is also very effective, by simply measuring the 3D volume of glass or liquid spheres at HPHT, thus providing density. This can be done in conjunction with the CAESAR technique and we illustrate this point. Finally, absorption profiles can be obtained via imaging techniques, providing another independent way to measure the density of these materials. References Y. Wang et al., A new technique for angle-dispersive powder diffraction using an energy-dispersive setup and synchrotron radiation (2004), J. Appl. Cryst. (2004). 37, 947-956 J. Philippe, Y. Le Godec, F. Bergame et M. Morand, Patent INPI 11 62335 (2013)

Hard X-ray irradiation of cosmic silicate analogs: structural evolution and astrophysical implications

NASA Astrophysics Data System (ADS)

Gavilan, L.; Jäger, C.; Simionovici, A.; Lemaire, J. L.; Sabri, T.; Foy, E.; Yagoubi, S.; Henning, T.; Salomon, D.; Martinez-Criado, G.

2016-03-01

Context. Protoplanetary disks, interstellar clouds, and active galactic nuclei contain X-ray-dominated regions. X-rays interact with the dust and gas present in such environments. While a few laboratory X-ray irradiation experiments have been performed on ices, X-ray irradiation experiments on bare cosmic dust analogs have been scarce up to now. Aims: Our goal is to study the effects of hard X-rays on cosmic dust analogs via in situ X-ray diffraction. By using a hard X-ray synchrotron nanobeam, we seek to simulate cumulative X-ray exposure on dust grains during their lifetime in these astrophysical environments and provide an upper limit on the effect of hard X-rays on dust grain structure. Methods: We prepared enstatite (MgSiO3) nanograins, which are analogs to cosmic silicates, via the melting-quenching technique. These amorphous grains were then annealed to obtain polycrystalline grains. These were characterized via scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) before irradiation. Powder samples were prepared in X-ray transparent substrates and were irradiated with hard X-rays nanobeams (29.4 keV) provided by beamline ID16B of the European Synchrotron Radiation Facility (Grenoble). X-ray diffraction images were recorded in transmission mode, and the ensuing diffractograms were analyzed as a function of the total X-ray exposure time. Results: We detected the amorphization of polycrystalline silicates embedded in an organic matrix after an accumulated X-ray exposure of 6.4 × 1027 eV cm-2. Pure crystalline silicate grains (without resin) do not exhibit amorphization. None of the amorphous silicate samples (pure and embedded in resin) underwent crystallization. We analyze the evolution of the polycrystalline sample embedded in an organic matrix as a function of X-ray exposure. Conclusions: Loss of diffraction peak intensity, peak broadening, and the disappearance of discrete spots and arcs reveal the amorphization of the resin embedded (originally polycrystalline) silicate sample. We explore the astrophysical implications of this laboratory result as an upper limit to the effect of X-rays on the structure of cosmic silicates.

Characterization of Metal Powders Used for Additive Manufacturing.

PubMed

Slotwinski, J A; Garboczi, E J; Stutzman, P E; Ferraris, C F; Watson, S S; Peltz, M A

2014-01-01

Additive manufacturing (AM) techniques can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process.

Energy resolution of the CdTe-XPAD detector: calibration and potential for Laue diffraction measurements on protein crystals.

PubMed

Medjoubi, Kadda; Thompson, Andrew; Bérar, Jean-François; Clemens, Jean-Claude; Delpierre, Pierre; Da Silva, Paulo; Dinkespiler, Bernard; Fourme, Roger; Gourhant, Patrick; Guimaraes, Beatriz; Hustache, Stéphanie; Idir, Mourad; Itié, Jean-Paul; Legrand, Pierre; Menneglier, Claude; Mercere, Pascal; Picca, Frederic; Samama, Jean-Pierre

2012-05-01

The XPAD3S-CdTe, a CdTe photon-counting pixel array detector, has been used to measure the energy and the intensity of the white-beam diffraction from a lysozyme crystal. A method was developed to calibrate the detector in terms of energy, allowing incident photon energy measurement to high resolution (approximately 140 eV), opening up new possibilities in energy-resolved X-ray diffraction. In order to demonstrate this, Laue diffraction experiments were performed on the bending-magnet beamline METROLOGIE at Synchrotron SOLEIL. The X-ray energy spectra of diffracted spots were deduced from the indexed Laue patterns collected with an imaging-plate detector and then measured with both the XPAD3S-CdTe and the XPAD3S-Si, a silicon photon-counting pixel array detector. The predicted and measured energy of selected diffraction spots are in good agreement, demonstrating the reliability of the calibration method. These results open up the way to direct unit-cell parameter determination and the measurement of high-quality Laue data even at low resolution. Based on the success of these measurements, potential applications in X-ray diffraction opened up by this type of technology are discussed.

Preliminary neutron diffraction analysis of challenging human manganese superoxide dismutase crystals

DOE PAGES

Azadmanesh, Jahaun; Trickel, Scott R.; Weiss, Kevin L.; ...

2017-03-29

Superoxide dismutases (SODs) are enzymes that protect against oxidative stress by dismutation of superoxide into oxygen and hydrogen peroxide through cyclic reduction and oxidation of the active-site metal. The complete enzymatic mechanisms of SODs are unknown since data on the positions of hydrogen are limited. Here, we present, methods for large crystal growth and neutron data collection of human manganese SOD (MnSOD) using perdeuteration and the MaNDi beamline at Oak Ridge National Laboratory. Furthermore, The crystal from which the human MnSOD data set was obtained is the crystal with the largest unit-cell edge (240 Å) from which data have beenmore » collectedvianeutron diffraction to sufficient resolution (2.30 Å) where hydrogen positions can be observed.« less

Multifit / Polydefix : a framework for the analysis of polycrystal deformation using X-rays

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

Merkel, Sébastien; Hilairet, Nadège

2015-06-27

Multifit/Polydefixis an open source IDL software package for the efficient processing of diffraction data obtained in deformation apparatuses at synchrotron beamlines.Multifitallows users to decompose two-dimensional diffraction images into azimuthal slices, fit peak positions, shapes and intensities, and propagate the results to other azimuths and images.Polydefixis for analysis of deformation experiments. Starting from output files created inMultifitor other packages, it will extract elastic lattice strains, evaluate sample pressure and differential stress, and prepare input files for further texture analysis. TheMultifit/Polydefixpackage is designed to make the tedious data analysis of synchrotron-based plasticity, rheology or other time-dependent experiments very straightforward and accessible tomore » a wider community.« less

Multipurpose end-station for coherent diffraction imaging and scattering at FERMI@Elettra free-electron laser facility.

PubMed

Capotondi, Flavio; Pedersoli, Emanuele; Bencivenga, Filippo; Manfredda, Michele; Mahne, Nicola; Raimondi, Lorenzo; Svetina, Cristian; Zangrando, Marco; Demidovich, Alexander; Nikolov, Ivaylo; Danailov, Miltcho; Masciovecchio, Claudio; Kiskinova, Maya

2015-05-01

The Diffraction and Projection Imaging (DiProI) beamline at FERMI, the Elettra free-electron laser (FEL), hosts a multi-purpose station that has been opened to users since the end of 2012. This paper describes the core capabilities of the station, designed to make use of the unique features of the FERMI-FEL for performing a wide range of static and dynamic scattering experiments. The various schemes for time-resolved experiments, employing both soft X-ray FEL and seed laser IR radiation are presented by using selected recent results. The ongoing upgrade is adding a reflection geometry setup for scattering experiments, expanding the application fields by providing both high lateral and depth resolution.

Preliminary neutron diffraction analysis of challenging human manganese superoxide dismutase crystals

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

Azadmanesh, Jahaun; Trickel, Scott R.; Weiss, Kevin L.

Superoxide dismutases (SODs) are enzymes that protect against oxidative stress by dismutation of superoxide into oxygen and hydrogen peroxide through cyclic reduction and oxidation of the active-site metal. The complete enzymatic mechanisms of SODs are unknown since data on the positions of hydrogen are limited. Here, we present, methods for large crystal growth and neutron data collection of human manganese SOD (MnSOD) using perdeuteration and the MaNDi beamline at Oak Ridge National Laboratory. Furthermore, The crystal from which the human MnSOD data set was obtained is the crystal with the largest unit-cell edge (240 Å) from which data have beenmore » collectedvianeutron diffraction to sufficient resolution (2.30 Å) where hydrogen positions can be observed.« less

Stability and melting of Fe3C at high pressure and temperature: Implication for the carbon in the Earth's core

NASA Astrophysics Data System (ADS)

Takahashi, S.; Ohtani, E.; Sakai, T.; Hirao, N.; Ohishi, Y.

2012-12-01

The Earth's core is regarded as an Fe-Ni alloy but its density is lower than that of pure Fe at the core conditions. Therefore, the Earth's core is supposed to contain light elements and carbon is one of the candidates of the light elements to explain the density deficit of the Earth's core. Nakajima et al. (2009) reported the melting temperature of Fe3C up to around 30 GPa based on textual observations, the chemical analysis of the quenched run products and in situ X-ray diffraction experiments using a Kawai-type multi anvil apparatus. Lord et al. (2009) reported melting temperatures of Fe3C up to 70 GPa, which was determined by the temperature plateau during increasing laser power using a laser-heated diamond anvil cell. They also suggested Fe+Fe7C3 is a stable subsolidus phase. There are obvious discrepancies between the melting curve and the stable subsolidus phase reported by Nakajima et al. (2009) and those reported by Lord et al. (2009). In this study, the melting temperatures of Fe3C and a subsolidus phase relation were determined based on in situ X-ray diffraction experiments. This study aims to reveal the stability field of Fe3C and the melting temperature of Fe3C and to discuss the behaviors of carbon in the Earth's core. We have performed experiments using a laser-heated diamond anvil cell combined with in situ X-ray diffraction experiment at BL10XU beamline, SPring-8 synchrotron facility. An NaCl powder and a rhenium or tungsten foil were used for the insulator and gasket, respectively. Melting of the sample was determined by disappearance of the X-ray diffraction peaks. We determined the melting relation of Fe3C up to 145 GPa by in situ X-ray diffraction experiments. Present results are close to Nakajima et al. (2009) up to 30 GPa but become close to that reported by Lord et al. (2009) at higher pressure conditions. The solidus temperature extrapolated to the ICB pressure, 330 GPa, is 5400 K. We also confirmed that Fe3C is stable as a subsolidus phase at least up to 237 GPa and 4100 K. This strongly suggests that Fe3C is a potential candidate of the Earth's inner core although we need further studies at the inner core conditions.

Crystal structure of choline fenofibrate (Trilipix®), (C5H14NO) (C17H14ClO4)

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

Kaduk, James A.; Zhong, Kai; Gindhart, Amy M.

2016-04-04

The crystal structure of choline fenofibrate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Choline fenofibrate crystallizes in space groupPbca(#61) witha= 12.341 03(2),b= 28.568 70(6),c= 12.025 62(2) Å,V= 4239.84(1) Å 3, andZ= 8. The hydroxyl group of the choline anion makes a strong hydrogen bond to the ionized carboxylate group of the fenofibrate anion. Together with C–H···O hydrogen bonds, these link the cations and anions into layers parallel to theac-plane. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™.

The BALDER Beamline at the MAX IV Laboratory

NASA Astrophysics Data System (ADS)

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

2016-05-01

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

The at-wavelength metrology facility for UV- and XUV-reflection and diffraction optics at BESSY-II

PubMed Central

Schäfers, F.; Bischoff, P.; Eggenstein, F.; Erko, A.; Gaupp, A.; Künstner, S.; Mast, M.; Schmidt, J.-S.; Senf, F.; Siewert, F.; Sokolov, A.; Zeschke, Th.

2016-01-01

A technology center for the production of high-precision reflection gratings has been established. Within this project a new optics beamline and a versatile reflectometer for at-wavelength characterization of UV- and XUV-reflection gratings and other (nano-) optical elements has been set up at BESSY-II. The Plane Grating Monochromator beamline operated in collimated light (c-PGM) is equipped with an SX700 monochromator, of which the blazed gratings (600 and 1200 lines mm−1) have been recently exchanged for new ones of improved performance produced in-house. Over the operating range from 10 to 2000 eV this beamline has very high spectral purity achieved by (i) a four-mirror arrangement of different coatings which can be inserted into the beam at different angles and (ii) by absorber filters for high-order suppression. Stray light and scattered radiation is removed efficiently by double sets of in situ exchangeable apertures and slits. By use of in- and off-plane bending-magnet radiation the beamline can be adjusted to either linear or elliptical polarization. One of the main features of a novel 11-axes reflectometer is the possibility to incorporate real life-sized gratings. The samples are adjustable within six degrees of freedom by a newly developed UHV-tripod system carrying a load up to 4 kg, and the reflectivity can be measured between 0 and 90° incidence angle for both s- and p-polarization geometry. This novel powerful metrology facility has gone into operation recently and is now open for external users. First results on optical performance and measurements on multilayer gratings will be presented here. PMID:26698047

CAT-ACT—A new highly versatile x-ray spectroscopy beamline for catalysis and radionuclide science at the KIT synchrotron light facility ANKA

NASA Astrophysics Data System (ADS)

Zimina, A.; Dardenne, K.; Denecke, M. A.; Doronkin, D. E.; Huttel, E.; Lichtenberg, H.; Mangold, S.; Pruessmann, T.; Rothe, J.; Spangenberg, Th.; Steininger, R.; Vitova, T.; Geckeis, H.; Grunwaldt, J.-D.

2017-11-01

CAT-ACT—the hard X-ray beamline for CATalysis and ACTinide/radionuclide research at the KIT synchrotron radiation facility ANKA—is dedicated to X-ray spectroscopy, including "flux hungry" photon-in/photon-out and correlative techniques and combines state-of-the-art optics with a unique infrastructure for radionuclide and catalysis research. Measurements can be performed at photon energies varying between 3.4 keV and 55 keV, thus encompassing the actinide M- and L-edge or potassium K-edge up to the K-edges of the lanthanide series such as cerium. Well-established X-ray absorption fine structure spectroscopy in transmission and fluorescence detection modes is available in combination with high energy-resolution X-ray emission spectroscopy or X-ray diffraction techniques. The modular beamline design with two alternately operated in-line experimental stations enables sufficient flexibility to adapt sample environments and detection systems to many scientific challenges. The ACT experimental station focuses on various aspects of nuclear waste disposal within the mission of the Helmholtz association to contribute to the solution of one of the greatest scientific and social challenges of our time—the safe disposal of heat producing, highly radioactive waste forms from nuclear energy production. It augments present capabilities at the INE-Beamline by increasing the flux and extending the energy range into the hard X-ray regime. The CAT experimental station focuses on catalytic materials, e.g., for energy-related and exhaust gas catalysis. Characterization of catalytically active materials under realistic reaction conditions and the development of in situ and operando cells for sample environments close to industrial reactors are essential aspects at CAT.

CAT-ACT-A new highly versatile x-ray spectroscopy beamline for catalysis and radionuclide science at the KIT synchrotron light facility ANKA.

PubMed

Zimina, A; Dardenne, K; Denecke, M A; Doronkin, D E; Huttel, E; Lichtenberg, H; Mangold, S; Pruessmann, T; Rothe, J; Spangenberg, Th; Steininger, R; Vitova, T; Geckeis, H; Grunwaldt, J-D

2017-11-01

CAT-ACT-the hard X-ray beamline for CATalysis and ACTinide/radionuclide research at the KIT synchrotron radiation facility ANKA-is dedicated to X-ray spectroscopy, including "flux hungry" photon-in/photon-out and correlative techniques and combines state-of-the-art optics with a unique infrastructure for radionuclide and catalysis research. Measurements can be performed at photon energies varying between 3.4 keV and 55 keV, thus encompassing the actinide M- and L-edge or potassium K-edge up to the K-edges of the lanthanide series such as cerium. Well-established X-ray absorption fine structure spectroscopy in transmission and fluorescence detection modes is available in combination with high energy-resolution X-ray emission spectroscopy or X-ray diffraction techniques. The modular beamline design with two alternately operated in-line experimental stations enables sufficient flexibility to adapt sample environments and detection systems to many scientific challenges. The ACT experimental station focuses on various aspects of nuclear waste disposal within the mission of the Helmholtz association to contribute to the solution of one of the greatest scientific and social challenges of our time-the safe disposal of heat producing, highly radioactive waste forms from nuclear energy production. It augments present capabilities at the INE-Beamline by increasing the flux and extending the energy range into the hard X-ray regime. The CAT experimental station focuses on catalytic materials, e.g., for energy-related and exhaust gas catalysis. Characterization of catalytically active materials under realistic reaction conditions and the development of in situ and operando cells for sample environments close to industrial reactors are essential aspects at CAT.

Mechanical behaviour of pressed and sintered CP Ti and Ti-6Al-7Nb alloy obtained from master alloy addition powder.

PubMed

Bolzoni, L; Weissgaerber, T; Kieback, B; Ruiz-Navas, E M; Gordo, E

2013-04-01

The Ti-6Al-7Nb alloy was obtained using the blending elemental approach with a master alloy and elemental titanium powders. Both the elemental titanium and the Ti-6Al-7Nb powders were characterised using X-ray diffraction, differential thermal analysis and dilatometry. The powders were processed using the conventional powder metallurgy route that includes uniaxial pressing and sintering. The trend of the relative density with the sintering temperature and the microstructural evolution of the materials sintered at different temperatures were analysed using scanning electron microscopy and X-ray diffraction. A minimum sintering temperature of 1200°C has to be used to ensure the homogenisation of the alloying elements and to obtain a pore structure composed of spherical pores. The sintered samples achieve relative density values that are typical for powder metallurgy titanium and no intermetallic phases were detected. Mechanical properties comparable to those specified for wrought Ti-6Al-7Nb medical devices are normally obtained. Therefore, the produced materials are promising candidates for load bearing applications as implant materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis of Amorphous Powders of Ni-Si and Co-Si Alloys by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Omuro, Keisuke; Miura, Harumatsu

1991-05-01

Amorphous powders of the Ni-Si and Co-Si alloys are synthesized by mechanical alloying (MA) from crystalline elemental powders using a high energy ball mill. The alloying and amorphization process is examined by X-ray diffraction, differential scanning calorimetry (DSC), and scanning electron microscopy. For the Ni-Si alloy, it is confirmed that the crystallization temperature of the MA powder, measured by DSC, is in good agreement with that of the powder sample prepared by mechanical grinding from the cast alloy ingot products of the same composition.

Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders.

PubMed

Yun, Yifeng; Zou, Xiaodong; Hovmöller, Sven; Wan, Wei

2015-03-01

Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED) data collection, namely automated diffraction tomography (ADT) and rotation electron diffraction (RED), have been developed. Compared with X-ray diffraction (XRD) and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD) provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni-Se-O-Cl crystals, zeolites, germanates, metal-organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three-dimensional ED methods will become crucially important in the near future.

High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

NASA Technical Reports Server (NTRS)

Palosz, B.; Stel'makh, S.; Grzanka, E.; Gierlotka, S.; Palosz, W.

2004-01-01

Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results of our studies show, that Sic nanocrystals have the features of two phases, each with its distinct elastic properties. and under pressures up to 8 GPa.

A Comparison of Cocrystal Structure Solutions from Powder and Single Crystal Techniques

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

S Lapidus; P Stephens; K Arora

We demonstrate the effectiveness and accuracy of high resolution powder diffraction for determination of cocrystal structures through a double-blind study. Structures of 10 cocrystals of varying complexity were determined independently using single crystal and powder techniques. The two methodologies give identical molecular packing and hydrogen bond topology, and an rms difference in covalent bond lengths of 0.035 {angstrom}. Powder techniques are clearly sufficient to establish a complete characterization of cocrystal geometry.

Heat-Stable Dry Powder Oxytocin Formulations for Delivery by Oral Inhalation.

PubMed

Fabio, Karine; Curley, Kieran; Guarneri, Joseph; Adamo, Benoit; Laurenzi, Brendan; Grant, Marshall; Offord, Robin; Kraft, Kelly; Leone-Bay, Andrea

2015-12-01

In this work, heat stable dry powders of oxytocin (OT) suitable for delivery by oral inhalation were prepared. The OT dry powders were prepared by spray drying using excipients chosen to promote OT stability including trehalose, isoleucine, polyvinylpyrrolidone, citrate (sodium citrate and citric acid), and zinc salts (zinc chloride and zinc citrate). Characterization by laser diffraction indicated that the OT dry powders had a median particle size of 2 μm, making them suitable for delivery by inhalation. Aerodynamic performance upon discharge from proprietary dry powder inhalers was evaluated by Andersen cascade impaction (ACI) and in an anatomically correct airway (ACA) model, and confirmed that the powders had excellent aerodynamic performance, with respirable fractions up to 77% (ACI, 30 L/min). Physicochemical characterization demonstrated that the powders were amorphous (X-ray diffraction) with high glass transition temperature (modulated differential scanning calorimetry, MDSC), suggesting the potential for stabilization of the OT in a glassy amorphous matrix. OT assay and impurity profile were conducted by reverse phase HPLC and liquid chromatography-mass spectrometry (LC-MS) after storage up to 32 weeks at 40°C/75%RH. Analysis demonstrated that OT dry powders containing a mixture of citrate and zinc salts retained more than 90% of initial assay after 32 weeks storage and showed significant reduction in dimers and trisulfide formation (up to threefold reduction compared to control).

X-ray investigations related to the shock history of the Shergotty achondrite

NASA Technical Reports Server (NTRS)

Horz, F.; Hanss, R.; Serna, C.

1986-01-01

The shock stress suffered by naturally shocked materials from the Shergotty achondrite was studied using X-ray diffraction techniques and experimentally shocked augite and enstatite as standards. The Shergotty pyroxenes revealed the formation of continuous diffraction rings, line broadening, preferred orientation of small scale diffraction domains, and other evidence of substantial lattice disorders. As disclosed by the application of Debye-Scherrer techniques, they are hybrids between single crystals and fine-grained random powders. The pyroxene lattice is very resistant to shock damage on smaller scales. While measurable lattice disaggregation and progressive fragmentation occur below 25 GPa, little additional damage is suffered from application of pressures between 30 to 60 GPa, making pressure calibration of naturally shocked pyroxenes via X-ray methods difficult. Powder diffractometer scans on pure maskelynite fractions of Shergotty revealed small amounts of still coherently diffracting plagioclase, which may contribute to the high refractive indices of the diaplectic feldspar glasses of Shergotty.

Examination of Short- and Long-Range Atomic Order Nanocrystalline SiC and Diamond by Powder Diffraction Methods

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Gierlotka, S.; Weber, H.-P.; Proffen, T.; Palosz, W.

2002-01-01

The real atomic structure of nanocrystals determines unique, key properties of the materials. Determination of the structure presents a challenge due to inherent limitations of standard powder diffraction techniques when applied to nanocrystals. Alternate methodology of the structural analysis of nanocrystals (several nanometers in size) based on Bragg-like scattering and called the "apparent lattice parameter" (alp) is proposed. Application of the alp methodology to examination of the core-shell model of nanocrystals will be presented. The results of application of the alp method to structural analysis of several nanopowders were complemented by those obtained by determination of the Atomic Pair Distribution Function, PDF. Based on synchrotron and neutron diffraction data measured in a large diffraction vector of up to Q = 25 Angstroms(exp -1), the surface stresses in nanocrystalline diamond and SiC were evaluated.

Valence fluctuating compound α-YbAlB4 studied by 174Yb Mössbauer spectroscopy and X-ray diffraction using synchrotron radiation

NASA Astrophysics Data System (ADS)

Oura, Momoko; Ikeda, Shugo; Masuda, Ryo; Kobayashi, Yasuhiro; Seto, Makoto; Yoda, Yoshitaka; Hirao, Naohisa; Kawaguchi, Saori I.; Ohishi, Yasuo; Suzuki, Shintaro; Kuga, Kentaro; Nakatsuji, Satoru; Kobayashi, Hisao

2018-05-01

The structural properties and the Yb 4 f electronic state of the valence fluctuating α-YbAlB4 have been investigated by powder X-ray diffraction under pressure and 174Yb Mössbauer spectroscopy with magnetic fields at low temperature, respectively, using synchrotron radiation. Powder X-ray diffraction patterns showed that the crystal structure does not change up to p ∼ 18 GPa at 8 K and the volume decreases smoothly. However, the pressure dependence of the difference in the structure factor between the (060) and (061) diffraction lines changes at ∼ 3.4 GPa, indicating the change of atomic coordination parameters. The 174Yb Mössbauer spectroscopy measurements at 2 K with 10 and 50 kOe suggest that the electrical quadrupole interaction changes by applied magnetic fields.

Synthesis and Characterization of Single-Source Molecular Precursors to Binary Metal Sulphides: Bis(Diethyldithiocarbamato) M(II)Trialkylphosphine (M=Zn and Cd) Adducts

DTIC Science & Technology

1994-05-06

while the heterobimetallic species, 7, thermally decomposed to give00 crystalline ZnO.5S according to X-ray powder diffraction data. A. SUBJECT TERMS 15... heterobimetallic species, 7, thermally decomposed to give crystalline ZnO.5CdO.5S according to X-ray powder diffraction data. LaGOSSIOn "or OTIS RA&I VT-iC TAB EU...on the NMR timescale, and a single heterobimetallic species. Attempts to distinguish these possibilities are described later. The variable temperature

Hydrothermal synthesis and characterization of hydroxyapatite and fluorhydroxyapatite nano-size powders.

PubMed

Montazeri, Leila; Javadpour, Jafar; Shokrgozar, Mohammad Ali; Bonakdar, Shahin; Javadian, Sayfoddin

2010-08-01

Pure hydroxyapatite (HAp) and fluoride-containing apatite powders (FHAp) were synthesized using a hydrothermal method. The powders were assessed by x-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscope (SEM) and F-selective electrode. X-ray diffraction results revealed the formation of single phase apatite structure for all the compositions synthesized in this work. However, the addition of a fluoride ion led to a systematic shift in the (3 0 0) peak of the XRD pattern as well as modifications in the FTIR spectra. It was found that the efficiency of fluoride ion incorporation decreased with the increase in the fluoride ion content. Fluorine incorporation efficiency was around 60% for most of the FHAp samples prepared in the current study. Smaller and less agglomerated particles were obtained by fluorine substitution. The bioactivity of the powder samples with different fluoride contents was compared by performing cell proliferation, alkaline phosphatase (ALP) and Alizarin red staining assays. Human osteoblast cells were used to assess the cellular responses to the powder samples in this study. Results demonstrated a strong dependence of different cell activities on the level of fluoridation.

Advanced Structural Analyses by Third Generation Synchrotron Radiation Powder Diffraction

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

Sakata, M.; Aoyagi, S.; Ogura, T.

2007-01-19

Since the advent of the 3rd generation Synchrotron Radiation (SR) sources, such as SPring-8, the capabilities of SR powder diffraction increased greatly not only in an accurate structure refinement but also ab initio structure determination. In this study, advanced structural analyses by 3rd generation SR powder diffraction based on the Large Debye-Scherrer camera installed at BL02B2, SPring-8 is described. Because of high angular resolution and high counting statistics powder data collected at BL02B2, SPring-8, ab initio structure determination can cope with a molecular crystals with 65 atoms including H atoms. For the structure refinements, it is found that a kindmore » of Maximum Entropy Method in which several atoms are omitted in phase calculation become very important to refine structural details of fairy large molecule in a crystal. It should be emphasized that until the unknown structure is refined very precisely, the obtained structure by Genetic Algorithm (GA) or some other ab initio structure determination method using real space structural knowledge, it is not possible to tell whether the structure obtained by the method is correct or not. In order to determine and/or refine crystal structure of rather complicated molecules, we cannot overemphasize the importance of the 3rd generation SR sources.« less

Investigation of the Surface Stress in SiC and Diamond Nanocrystals by In-situ High Pressure Powder Diffraction Technique

NASA Technical Reports Server (NTRS)

Palosz, B.; Stelmakh, S.; Grzanka, E.; Gierlotka, S.; Zhao, Y.; Palosz, W.

2003-01-01

The real atomic structure of nanocrystals determines key properties of the materials. For such materials the serious experimental problem lies in obtaining sufficiently accurate measurements of the structural parameters of the crystals, since very small crystals constitute rather a two-phase than a uniform crystallographic phase system. As a result, elastic properties of nanograins may be expected to reflect a dual nature of their structure, with a corresponding set of different elastic property parameters. We studied those properties by in-situ high-pressure powder diffraction technique. For nanocrystalline, even one-phase materials such measurements are particularly difficult to make since determination of the lattice parameters of very small crystals presents a challenge due to inherent limitations of standard elaboration of powder diffractograms. In this investigation we used our methodology of the structural analysis, the 'apparent lattice parameter' (alp) concept. The methodology allowed us to avoid the traps (if applied to nanocrystals) of standard powder diffraction evaluation techniques. The experiments were performed for nanocrystalline Sic and GaN powders using synchrotron sources. We applied both hydrostatic and isostatic pressures in the range of up to 40 GPa. Elastic properties of the samples were examined based on the measurements of a change of the lattice parameters with pressure. The results show a dual nature of the mechanical properties (compressibilities) of the materials, indicating a complex, core-shell structure of the grains.

RoboDiff: combining a sample changer and goniometer for highly automated macromolecular crystallography experiments

PubMed Central

Nurizzo, Didier; Bowler, Matthew W.; Caserotto, Hugo; Dobias, Fabien; Giraud, Thierry; Surr, John; Guichard, Nicolas; Papp, Gergely; Guijarro, Matias; Mueller-Dieckmann, Christoph; Flot, David; McSweeney, Sean; Cipriani, Florent; Theveneau, Pascal; Leonard, Gordon A.

2016-01-01

Automation of the mounting of cryocooled samples is now a feature of the majority of beamlines dedicated to macromolecular crystallography (MX). Robotic sample changers have been developed over many years, with the latest designs increasing capacity, reliability and speed. Here, the development of a new sample changer deployed at the ESRF beamline MASSIF-1 (ID30A-1), based on an industrial six-axis robot, is described. The device, named RoboDiff, includes a high-capacity dewar, acts as both a sample changer and a high-accuracy goniometer, and has been designed for completely unattended sample mounting and diffraction data collection. This aim has been achieved using a high level of diagnostics at all steps of the process from mounting and characterization to data collection. The RoboDiff has been in service on the fully automated endstation MASSIF-1 at the ESRF since September 2014 and, at the time of writing, has processed more than 20 000 samples completely automatically. PMID:27487827

Calculating cellulose diffraction patterns

USDA-ARS?s Scientific Manuscript database

Although powder diffraction of cellulose is a common experiment, the patterns are not widely understood. The theory is mathematical, there are numerous different crystal forms, and the conventions are not standardized. Experience with IR spectroscopy is not directly transferable. An awful error, tha...

Titration of a Solid Acid Monitored by X-Ray Diffraction

ERIC Educational Resources Information Center

Dungey, Keenan E.; Epstein, Paul

2007-01-01

An experiment is described to introduce students to an important class of solid-state reactions while reinforcing concepts of titration by using a pH meter and a powder X-ray diffractometer. The experiment was successful in teaching students the abstract concepts of solid-state structure and diffraction by applying the diffraction concepts learned…

Characterization of Metal Powders Used for Additive Manufacturing

PubMed Central

Slotwinski, JA; Garboczi, EJ; Stutzman, PE; Ferraris, CF; Watson, SS; Peltz, MA

2014-01-01

Additive manufacturing (AM) techniques1 can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process. PMID:26601040

Structure of N-(5-ethyl-[1,3,4]-thiadiazole-2-yl)toluenesulfonamide by combined X-ray powder diffraction, 13C solid-state NMR and molecular modelling.

PubMed

Hangan, Adriana; Borodi, Gheorghe; Filip, Xenia; Tripon, Carmen; Morari, Cristian; Oprean, Luminita; Filip, Claudiu

2010-12-01

The crystal structure solution of the title compound is determined from microcrystalline powder using a multi-technique approach that combines X-ray powder diffraction (XRPD) data analysis based on direct-space methods with information from (13)C solid-state NMR (SSNMR), and molecular modelling using the GIPAW (gauge including projector augmented-wave) method. The space group is Pbca with one molecule in the asymmetric unit. The proposed methodology proves very useful for unambiguously characterizing the supramolecular arrangement adopted by the N-(5-ethyl-[1,3,4]-thiadiazole-2-yl)toluenesulfonamide molecules in the crystal, which consists of extended double strands held together by C-H···π non-covalent interactions.

Crystal structure of paliperidone palmitate (INVEGA SUSTENNA®), C39H57FN4O4

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

Kaduk, James A.; Dmitrienko, Artem O.; Gindhart, Amy M.

2017-08-29

The crystal structure of paliperidone palmitate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Paliperidone palmitate crystallizes in space groupP2 1/c(#14) witha= 34.415 40(35),b= 10.093 49(7),c= 10.904 92(9) Å,β= 94.3917(9)°,V= 3776.94(6) Å 3, andZ= 4. The conformation of the paliperidone fragment differs from that of the parent compound. The palmitate chain exhibits a slight twist close to the ester group. Several C–H•••O hydrogen bonds contribute to the crystal packing, which is dominated by van der Waals interactions. The powder pattern is included in the Powder Diffraction File™ as entry 00-066-1614.

Bragg coherent diffraction imaging and metrics for radiation damage in protein micro-crystallography.

PubMed

Coughlan, H D; Darmanin, C; Kirkwood, H J; Phillips, N W; Hoxley, D; Clark, J N; Vine, D J; Hofmann, F; Harder, R J; Maxey, E; Abbey, B

2017-01-01

The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals (Helliwell, 1984). Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to the diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. A possible mechanism to account for these observations is proposed.

Bragg coherent diffraction imaging and metrics for radiation damage in protein micro-crystallography

DOE PAGES

Coughlan, H. D.; Darmanin, C.; Kirkwood, H. J.; ...

2017-01-01

The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals. Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to themore » diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. As a result, a possible mechanism to account for these observations is proposed.« less

Bragg coherent diffraction imaging and metrics for radiation damage in protein micro-crystallography

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

Coughlan, H. D.; Darmanin, C.; Kirkwood, H. J.

The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals. Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to themore » diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. As a result, a possible mechanism to account for these observations is proposed.« less

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Luo, S. N.; Jensen, B. J.; Hooks, D. E.; Fezzaa, K.; Ramos, K. J.; Yeager, J. D.; Kwiatkowski, K.; Shimada, T.

2012-07-01

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (˜2 μm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.

Nonvolatile RRAM cells from polymeric composites embedding recycled SiC powders.

PubMed

De Girolamo Del Mauro, Anna; Nenna, Giuseppe; Miscioscia, Riccardo; Freda, Cesare; Portofino, Sabrina; Galvagno, Sergio; Minarini, Carla

2014-10-21

Silicon carbide powders have been synthesized from tires utilizing a patented recycling process. Dynamic light scattering, Raman spectroscopy, SEM microscopy, and X-ray diffraction have been carried out to gather knowledge about powders and the final composite structure. The obtained powder has been proven to induce resistive switching in a PMMA polymer-based composite device. Memory effect has been detected in two-terminal devices having coplanar contacts and quantified by read-write-erase measurements in terms of level separation and persistence.

Same Precursor, Two Different Products: Comparing the Structural Evolution of In–Ga–O “Gel-Derived” Powders and Solution-Cast Films Using Pair Distribution Function Analysis

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

Wood, Suzannah R.; Woods, Keenan N.; Plassmeyer, Paul N.

Amorphous metal oxides are central to a variety of technological applications. In particular, indium gallium oxide has garnered attention as a thin-film transistor channel layer material. In this work we examine the structural evolution of indium gallium oxide gel-derived powders and thin films using infrared vibrational spectroscopy, X-ray diffraction, and pair distribution function (PDF) analysis of X-ray total scattering from standard and normal incidence thin-film geometries (tfPDF). We find that the gel-derived powders and films from the same aqueous precursor evolve differently with temperature, forming mixtures of Ga-substituted In2O3 and In-substituted β-Ga2O3 with different degrees of substitution. X-ray total scatteringmore » and PDF analysis indicate that the majority phase for both the powders and films is an amorphous/nanocrystalline β-Ga2O3 phase, with a minor constituent of In2O3 with significantly larger coherence lengths. This amorphous β-Ga2O3 phase could not be identified using the conventional Bragg diffraction techniques traditionally used to study crystalline metal oxide thin films. The combination of Bragg diffraction and tfPDF provides a much more complete description of film composition and structure, which can be used to detail the effect of processing conditions and structure–property relationships. This study also demonstrates how structural features of amorphous materials, traditionally difficult to characterize by standard diffraction, can be elucidated using tfPDF.« less

Synthesis and characterization of graphene oxide using modified Hummer's method

NASA Astrophysics Data System (ADS)

Kaur, Manpreet; Kaur, Harsimran; Kukkar, Deepak

2018-05-01

In the present study, a simple approach has been followed for the synthesis of graphene oxide (GO) using modified Hummers method in which graphite powder was oxidized in the presence of concentrated H2SO4 and KMnO4. The amount of NaNO3 and KMnO4 was varied to produce sheet like structure. The varied concentrations of NaNO3 and KMnO4 resulted in yielding large amount of the product. Structural, morphological and physicochemical features of the product were studied using UV-Visible spectrophotometer, Fourier Transform infrared spectroscopy (FTIR), and crystal structure was determined using X-ray powder diffraction (XRD). UV-Vis spectra of GO was observed at a maximum absorption of 230 nm due to (π-π*) transition of atomic carbon-carbon bonds. FTIR spectra revealed the presence of oxygen containing functional groups which ensures the complete exfoliation of graphite into graphene oxide X-ray powder diffraction pattern of the product showed the diffraction peak at (2θ = 26.7°) with an interlayer spacing of 0.334 nm. All the above characterizations successfully confirmed the formation of GO.

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

Aldridge, James D.; Womick, Jordan M.; Rosmus, Kimberly A.

Novel quaternary lanthanide-substituted oxides of stoichiometry LnxY2-xTi2O7 (where Ln is lanthanum, neodymium, samarium, gadolinium, or ytterbium) were prepared by traditional high-temperature, solid-state techniques and characterized by X-ray powder diffraction. Samples with nominal values of x up to 1.0 were attempted. The well-studied ternary cubic pyrochlore compound yttrium titanium oxide (Y2Ti2O7, space group Fd-3m, Z = 8), served as a parent structural framework in which Ln3+ cations were substituted on the Y3+ site. Laboratory-grade X-ray powder diffraction data revealed pure quaternary pyrochlore phases for LnxY2-xTi2O7 with x ≤ 0.2. Pyrochlore phase purity was verified by Rietveld analysis using high-resolution synchrotron X-raymore » powder diffraction data when x ≤ 0.2, however, for La3+ substitution specifically, pure quaternary pyrochlore formed at x<0.1. Band gap energies on selected samples were determined using optical diffuse reflectance spectroscopy and showed that these materials can be classified as electrical insulators with indirect band gap energies around 3.7 eV.« less

Real-time monitoring of laser powder bed fusion process using high-speed X-ray imaging and diffraction

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

Zhao, Cang; Fezzaa, Kamel; Cunningham, Ross W.

Here, we employ the high-speed synchrotron hard X-ray imaging and diffraction techniques to monitor the laser powder bed fusion (LPBF) process of Ti-6Al-4V in situ and in real time. We demonstrate that many scientifically and technologically significant phenomena in LPBF, including melt pool dynamics, powder ejection, rapid solidification, and phase transformation, can be probed with unprecedented spatial and temporal resolutions. In particular, the keyhole pore formation is experimentally revealed with high spatial and temporal resolutions. The solidification rate is quantitatively measured, and the slowly decrease in solidification rate during the relatively steady state could be a manifestation of the recalescencemore » phenomenon. The high-speed diffraction enables a reasonable estimation of the cooling rate and phase transformation rate, and the diffusionless transformation from β to α’ phase is evident. The data present here will facilitate the understanding of dynamics and kinetics in metal LPBF process, and the experiment platform established will undoubtedly become a new paradigm for future research and development of metal additive manufacturing.« less

Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

NASA Astrophysics Data System (ADS)

Cheung, Eugene Y.; David, Sarah E.; Harris, Kenneth D. M.; Conway, Barbara R.; Timmins, Peter

2007-03-01

We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H 2NC(CH 3) 3-n(CH 2OH) n, with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family ( n=0, 1, 2), but significantly contrasting structural properties for the member with n=3.

Real-time monitoring of laser powder bed fusion process using high-speed X-ray imaging and diffraction

DOE PAGES

Zhao, Cang; Fezzaa, Kamel; Cunningham, Ross W.; ...

2017-06-15

Here, we employ the high-speed synchrotron hard X-ray imaging and diffraction techniques to monitor the laser powder bed fusion (LPBF) process of Ti-6Al-4V in situ and in real time. We demonstrate that many scientifically and technologically significant phenomena in LPBF, including melt pool dynamics, powder ejection, rapid solidification, and phase transformation, can be probed with unprecedented spatial and temporal resolutions. In particular, the keyhole pore formation is experimentally revealed with high spatial and temporal resolutions. The solidification rate is quantitatively measured, and the slowly decrease in solidification rate during the relatively steady state could be a manifestation of the recalescencemore » phenomenon. The high-speed diffraction enables a reasonable estimation of the cooling rate and phase transformation rate, and the diffusionless transformation from β to α’ phase is evident. The data present here will facilitate the understanding of dynamics and kinetics in metal LPBF process, and the experiment platform established will undoubtedly become a new paradigm for future research and development of metal additive manufacturing.« less

Raman scattering and X-ray powder diffraction studies of hydrate layered perovskites: dirubidium aquapentafluoromanganate(III) and dipotassium aquapentafluoroferrate(III)

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

Galicka, Karolina; Slodczyk, Aneta; Ratuszna, Alicja

2004-06-08

The structural and vibrational properties of above mentioned crystals were determined using X-ray powder diffraction and Raman scattering experiments. At room temperature hydrate layered perovskites: Rb{sub 2}MnF{sub 5}{center_dot}H{sub 2}O and K{sub 2}FeF{sub 5}{center_dot}H{sub 2}O exhibit orthorhombic--Cmcm (D{sub 2h}{sup 17}) and monoclinic--C2/c (C{sub 2h}{sup 6}) symmetry. Their structure is built up of MnF{sub 6} or FeF{sub 5}{center_dot}H{sub 2}O octahedra forming trans-linked zig-zag chains or hydrogen bonded zig-zag chains along the major crystallographic direction [0 0 1], respectively. To confirm crystal structures and to describe lattice dynamics of these compounds the vibrational normal modes (in {gamma} point of first Brillouin zone) weremore » calculated on the base of the group theory analysis and compared with the spectra obtained from Raman scattering experiments. A relatively good reliability was obtained for both X-ray powder diffraction and Raman scattering.« less

Investigation of phase evolution of CaCu3Ti4O12 (CCTO) by in situ synchrotron high-temperature powder diffraction

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Huang, Saifang; Zhang, Weijun; Cao, Peng; Huang, Zhaohui; Gao, Wei

2014-03-01

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu3Ti4O12 (CCTO) precursors prepared via solid-state and sol-gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol-gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol-gel precursor. Both precursors are able to be calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study.

Development of Cu Reinforced SiC Particulate Composites

NASA Astrophysics Data System (ADS)

Singh, Harshpreet; Kumar, Lailesh; Nasimul Alam, Syed

2015-02-01

This paper presents the results of Cu-SiCp composites developed by powder metallurgy route and an attempt has been made to make a comparison between the composites developed by using unmilled Cu powder and milled Cu powder. SiC particles as reinforcement was blended with unmilled and as-milled Cu powderwith reinforcement contents of 10, 20, 30, 40 vol. % by powder metallurgy route. The mechanical properties of pure Cu and the composites developed were studied after sintering at 900°C for 1 h. Density of the sintered composites were found out based on the Archimedes' principle. X-ray diffraction of all the composites was done in order to determine the various phases in the composites. Scanning electron microscopy (SEM) and EDS (electron diffraction x-ray spectroscopy) was carried out for the microstructural analysis of the composites. Vickers microhardness tester was used to find out the hardness of the samples. Wear properties of the developed composites were also studied.

Application of Powder Diffraction Methods to the Analysis of Short- and Long-Range Atomic Order in Nanocrystalline Diamond and SiC: The Concept of the Apparent Lattice Parameter (alp)

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Gierlotka, S.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Weber, H.-P.; Palosz, W.

2003-01-01

Two methods of the analysis of powder diffraction patterns of diamond and SiC nanocrystals are presented: (a) examination of changes of the lattice parameters with diffraction vector Q ('apparent lattice parameter', alp) which refers to Bragg scattering, and (b), examination of changes of inter-atomic distances based on the analysis of the atomic Pair Distribution Function, PDF. Application of these methods was studied based on the theoretical diffraction patterns computed for models of nanocrystals having (i) a perfect crystal lattice, and (ii), a core-shell structure, i.e. constituting a two-phase system. The models are defined by the lattice parameter of the grain core, thickness of the surface shell, and the magnitude and distribution of the strain field in the shell. X-ray and neutron experimental diffraction data of nanocrystalline SiC and diamond powders of the grain diameter from 4 nm up to micrometers were used. The effects of the internal pressure and strain at the grain surface on the structure are discussed based on the experimentally determined dependence of the alp values on the Q-vector, and changes of the interatomic distances with the grain size determined experimentally by the atomic Pair Distribution Function (PDF) analysis. The experimental results lend a strong support to the concept of a two-phase, core and the surface shell structure of nanocrystalline diamond and SiC.

Far-Field High-Energy Diffraction Microscopy: A Non-Destructive Tool for Characterizing the Microstructure and Micromechanical State of Polycrystalline Materials

DOE PAGES

Park, Jun-Sang; Zhang, Xuan; Kenesei, Peter; ...

2017-08-31

A suite of non-destructive, three-dimensional X-ray microscopy techniques have recently been developed and used to characterize the microstructures of polycrystalline materials. These techniques utilize high-energy synchrotron radiation and include near-field and far-field diffraction microscopy (NF- and FF-HEDM, respectively) and absorption tomography. Several compatible sample environments have also been developed, enabling a wide range of 3D studies of material evolution. In this article, the FF-HEDM technique is described in detail, including its implementation at the 1-ID beamline of the Advanced Photon Source. Examples of how the information obtained from FF-HEDM can be used to deepen our understanding of structure-property-processing relationships inmore » selected materials are presented.« less

A general method for baseline-removal in ultrafast electron powder diffraction data using the dual-tree complex wavelet transform.

PubMed

René de Cotret, Laurent P; Siwick, Bradley J

2017-07-01

The general problem of background subtraction in ultrafast electron powder diffraction (UEPD) is presented with a focus on the diffraction patterns obtained from materials of moderately complex structure which contain many overlapping peaks and effectively no scattering vector regions that can be considered exclusively background. We compare the performance of background subtraction algorithms based on discrete and dual-tree complex (DTCWT) wavelet transforms when applied to simulated UEPD data on the M1-R phase transition in VO 2 with a time-varying background. We find that the DTCWT approach is capable of extracting intensities that are accurate to better than 2% across the whole range of scattering vector simulated, effectively independent of delay time. A Python package is available.

In Situ Neutron Diffraction of Rare-Earth Phosphate Proton Conductors Sr/Ca-doped LaPO4 at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Al-Wahish, Amal; Al-Binni, Usama; Bridges, C. A.; Huq, A.; Bi, Z.; Paranthaman, M. P.; Tang, S.; Kaiser, H.; Mandrus, D.

Acceptor-doped lanthanum orthophosphates are potential candidate electrolytes for proton ceramic fuel cells. We combined neutron powder diffraction (NPD) at elevated temperatures up to 800° C , X-ray powder diffraction (XRD) and scanning electron microscopy (SEM) to investigate the crystal structure, defect structure, thermal stability and surface topography. NPD shows an average bond length distortion in the hydrated samples. We employed Quasi-Elastic Neutron Scattering (QENS) and electrochemical impedance spectroscopy (EIS) to study the proton dynamics of the rare-earth phosphate proton conductors 4.2% Sr/Ca-doped LaPO4. We determined the bulk diffusion and the self-diffusion coefficients. Our results show that QENS and EIS are probing fundamentally different proton diffusion processes. Supported by the U.S. Department of Energy.

X-ray diffraction study of the caged magnetic compound DyFe 2 Zn 20 at low temperatures

NASA Astrophysics Data System (ADS)

Ohashi, M.; Ohashi, K.; Sawabu, M.; Miyagawa, M.; Maeta, K.; Isikawa, Y.

2018-05-01

We have carried out high-angle X-ray powder diffraction measurements of the caged magnetic compound DyFe2Zn20 at low temperature between 14 and 300 K. Even though a strong magnetic anisotropy exists in the magnetization and magnetic susceptibility due to strong exchange interaction between Fe and Dy, almost all X-ray powder diffraction peaks correspond to Bragg reflections of the cubic structural models not only at room temperature paramagnetic state but also at low temperature magnetic ordering state. The Debye temperature is obtained to be 227 K from the results of the volumetric thermal expansion coefficient, which is approximately coincident with that of CeRu2Zn20 (245 K) and that of pure Zn metal (235 K).

AutoDrug: fully automated macromolecular crystallography workflows for fragment-based drug discovery

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

Tsai, Yingssu; Stanford University, 333 Campus Drive, Mudd Building, Stanford, CA 94305-5080; McPhillips, Scott E.

New software has been developed for automating the experimental and data-processing stages of fragment-based drug discovery at a macromolecular crystallography beamline. A new workflow-automation framework orchestrates beamline-control and data-analysis software while organizing results from multiple samples. AutoDrug is software based upon the scientific workflow paradigm that integrates the Stanford Synchrotron Radiation Lightsource macromolecular crystallography beamlines and third-party processing software to automate the crystallography steps of the fragment-based drug-discovery process. AutoDrug screens a cassette of fragment-soaked crystals, selects crystals for data collection based on screening results and user-specified criteria and determines optimal data-collection strategies. It then collects and processes diffraction data,more » performs molecular replacement using provided models and detects electron density that is likely to arise from bound fragments. All processes are fully automated, i.e. are performed without user interaction or supervision. Samples can be screened in groups corresponding to particular proteins, crystal forms and/or soaking conditions. A single AutoDrug run is only limited by the capacity of the sample-storage dewar at the beamline: currently 288 samples. AutoDrug was developed in conjunction with RestFlow, a new scientific workflow-automation framework. RestFlow simplifies the design of AutoDrug by managing the flow of data and the organization of results and by orchestrating the execution of computational pipeline steps. It also simplifies the execution and interaction of third-party programs and the beamline-control system. Modeling AutoDrug as a scientific workflow enables multiple variants that meet the requirements of different user groups to be developed and supported. A workflow tailored to mimic the crystallography stages comprising the drug-discovery pipeline of CoCrystal Discovery Inc. has been deployed and successfully demonstrated. This workflow was run once on the same 96 samples that the group had examined manually and the workflow cycled successfully through all of the samples, collected data from the same samples that were selected manually and located the same peaks of unmodeled density in the resulting difference Fourier maps.« less

Nanometer-scale characterization of laser-driven plasmas, compression, shocks and phase transitions, by coherent small angle x-ray scattering

NASA Astrophysics Data System (ADS)

Kluge, Thomas

2015-11-01

Combining ultra-intense short-pulse and high-energy long-pulse lasers, with brilliant coherent hard X-ray FELs, such as the Helmholtz International Beamline for Extreme Fields (HIBEF) under construction at the HED Instrument of European XFEL, or MEC at LCLS, holds the promise to revolutionize our understanding of many High Energy Density Physics phenomena. Examples include the relativistic electron generation, transport, and bulk plasma response, and ionization dynamics and heating in relativistic laser-matter interactions, or the dynamics of laser-driven shocks, quasi-isentropic compression, and the kinetics of phase transitions at high pressure. A particularly promising new technique is the use of coherent X-ray diffraction to characterize electron density correlations, and by resonant scattering to characterize the distribution of specific charge-state ions, either on the ultrafast time scale of the laser interaction, or associated with hydrodynamic motion. As well one can image slight density changes arising from phase transitions inside of shock-compressed high pressure matter. The feasibility of coherent diffraction techniques in laser-driven matter will be discussed. including recent results from demonstration experiments at MEC. Among other things, very sharp density changes from laser-driven compression are observed, having an effective step width of 10 nm or smaller. This compares to a resolution of several hundred nm achievedpreviously with phase contrast imaging. and on behalf of HIBEF User Consortium, for the Helmholtz International Beamline for Extreme Fields at the European XFEL.

Beamline Electrostatic Levitator (BESL) for in-situ High Energy K-Ray Diffraction Studies of Levitated Solids and Liquids at High Temperature

NASA Technical Reports Server (NTRS)

Gangopadhyay, A. K.; Lee, G. W.; Kelton, K. F.; Rogers, J. R.; Goldman, A. I.; Robinson, D. S.; Rathz, T. J.; Hyers, R. W.

2005-01-01

Determinations of the phase formation sequence, the crystal structures and the thermodynamic properties of materials at high temperatures are difficult because of contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic (EML), aerodynamic, and acoustic levitation, are most suitable these studies. An adaptation of ESL for in-situ structural studies of a wide range of materials, including metals, semiconductors, insulators using high energy (125 keV) synchrotron x-rays is described here. This beamline ESL (BESL) allows the in-situ determination of the atomic structures of equilibrium solid and liquid phases, including undercooled liquids, as well as real-time studies of solid-solid and liquid-solid phase transformations. The use of image plate (MAR345) or GE-Angio detectors enables fast (30 ms - 1s) acquisition of complete diffraction patterns over a wide q-range (4 - 140/mm). The wide temperature range (300 - 2500 K), containerless processing under high vacuum (10(exp -7) - 10(exp -8) torr), and fast data acquisition, make BESL particularly suitable for phase diagram studies of high temperature materials. An additional, critically important, feature of BESL is the ability to also make simultaneous measurement of a host of thermo-physical properties, including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension; all on the same sample and simultaneous with the structural measurements.

Development of a novel dry powder inhalation formulation for the delivery of rivastigmine hydrogen tartrate.

PubMed

Simon, Alice; Amaro, Maria Inês; Cabral, Lucio Mendes; Healy, Anne Marie; de Sousa, Valeria Pereira

2016-03-30

The purpose of this study was to prepare engineered particles of rivastigmine hydrogen tartrate (RHT) and to characterize the physicochemical and aerodynamic properties, in comparison to a lactose carrier formulation (LCF). Microparticles were prepared from ethanol/water solutions containing RHT with and without the incorporation of L-leucine (Leu), using a spray dryer. Dry powder inhaler formulations prepared were characterized by scanning electron microscopy, powder X-ray diffraction, laser diffraction particle sizing, ATR-FTIR, differential scanning calorimetry, bulk and tapped density, dynamic vapour sorption and in vitro aerosol deposition behaviour using a next generation impactor. The smooth-surfaced spherical morphology of the spray dried microparticles was altered by adding Leu, resulting in particles becoming increasingly wrinkled with increasing Leu. Powders presented low densities. The glass transition temperature was sufficiently high (>90 °C) to suggest good stability at room temperature. As Leu content increased, spray dried powders presented lower residual solvent content, lower particle size, higher fine particle fraction (FPF<5 μm), and lower mass median aerodynamic diameter (MMAD). The LCF showed a lower FPF and higher MMAD, relative to the spray dried formulations containing more than 10% Leu. Spray dried RHT powders presented better aerodynamic properties, constituting a potential drug delivery system for oral inhalation. Copyright © 2016. Published by Elsevier B.V.

Neutron powder diffraction studies as a function of temperature of structure II hydrate formed from propane

USGS Publications Warehouse

Rawn, C.J.; Rondinone, A.J.; Chakoumakos, B.C.; Circone, S.; Stern, L.A.; Kirby, S.H.; Ishii, Y.

2003-01-01

Neutron powder diffraction data confirm that hydrate samples synthesized with propane crystallize as structure type II hydrate. The structure has been modeled using rigid-body constraints to describe C3H8 molecules located in the eight larger polyhedral cavities of a deuterated host lattice. Data were collected at 12, 40, 100, 130, 160, 190, 220, and 250 K and used to calculate the thermal expansivity from the temperature dependence of the lattice parameters. The data collected allowed for full structural refinement of atomic coordinates and the atomic-displacement parameters.

TSX-PLUS MULTI-TASKING UPGRADE FOR THE NICOLET L-11 POWDER DIFFRACTION SYSTEM.

USGS Publications Warehouse

Fitzpatrick, J.; Queen, David L.

1985-01-01

In August of 1982, a single-user, dual-translator, automated powder diffraction system was purchased by the Denver Research Institute for use on project work in the Chemical and Materials Sciences Division. Within a short period of time, the system had already become saturated with users. Scheduling conflicts arose. In view of these problems, an answer was sought in the form of hardware and software changes which would allow many users access to the system simultaneously. A low-cost, minimum impact solution was eventually found. The elements of the solution are reported.

Structure resolution by electron diffraction tomography of the complex layered iron-rich Fe-2234-type Sr{sub 5}Fe{sub 6}O{sub 15.4}

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

Lepoittevin, Christophe, E-mail: christophe.lepoittevin@neel.cnrs.fr

2016-10-15

The crystal structure of the strontium ferrite Sr{sub 5}Fe{sub 6}O{sub 15.4}, was solved by direct methods on electron diffraction tomography data acquired on a transmission electron microscope. The refined cell parameters are a=27.4047(3) Å, b=5.48590(7) Å and c=42.7442(4) Å in Fm2m symmetry. Its structure is built up from the intergrowth sequence between a quadruple perovskite-type layer with a complex rock-salt (RS)-type block. In the latter iron atoms are found in two different environments : tetragonal pyramid and tetrahedron. The structural model was refined by Rietveld method based on the powder X-ray diffraction pattern. - Highlights: • Complex structure of Sr{submore » 5}Fe{sub 6}O{sub 15.4} solved by electron diffraction tomography. • Observed Fourier maps allow determining missing oxygen atoms in the structure. • Structural model refined from powder X-ray diffraction data. • Intergrowth between quadruple perovskite layer with double rock-salt-type layer.« less

Idealized powder diffraction patterns for cellulose polymorphs

USDA-ARS?s Scientific Manuscript database

Cellulose samples are routinely analyzed by X-ray diffraction to determine their crystal type (polymorph) and crystallinity. However, the connection is seldom made between those efforts and the crystal structures of cellulose that have been determined with synchrotron X-radiation and neutron diffrac...

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

Gao, Xiong-Zhuo; National Laboratory of Protein Engineering and Plant Genetic Engineering, College of Life Sciences, Peking University, Beijing 100871; Li, Lan-Fen

The SMU.961 protein from S. mutans was crystallized and preliminary characterization of the crystals, which diffracted to 2.9 Å resolution, shows them to belong to space group C2. The smu.961 gene encodes a putative protein of 183 residues in Streptococcus mutans, a major pathogen in human dental caries. The gene was cloned into expression vector pET28a and expressed in a substantial quantity in Escherichia coli strain BL21 (DE3) with a His tag at its N-terminus. The recombinant protein SMU.961 was purified to homogeneity in a two-step procedure consisting of Ni{sup 2+}-chelating and size-exclusion chromatography. Crystals suitable for X-ray diffraction weremore » obtained by the hanging-drop vapour-diffusion method and diffracted to 2.9 Å resolution at beamline I911-3, MAX-II-lab, Sweden. The crystal belonged to space group C2, with unit-cell parameters a = 98.62, b = 73.73, c = 184.73 Å, β = 98.82°.« less

Quantitative analysis of crystalline pharmaceuticals in powders and tablets by a pattern-fitting procedure using X-ray powder diffraction data.

PubMed

Yamamura, S; Momose, Y

2001-01-16

A pattern-fitting procedure for quantitative analysis of crystalline pharmaceuticals in solid dosage forms using X-ray powder diffraction data is described. This method is based on a procedure for pattern-fitting in crystal structure refinement, and observed X-ray scattering intensities were fitted to analytical expressions including some fitting parameters, i.e. scale factor, peak positions, peak widths and degree of preferred orientation of the crystallites. All fitting parameters were optimized by the non-linear least-squares procedure. Then the weight fraction of each component was determined from the optimized scale factors. In the present study, well-crystallized binary systems, zinc oxide-zinc sulfide (ZnO-ZnS) and salicylic acid-benzoic acid (SA-BA), were used as the samples. In analysis of the ZnO-ZnS system, the weight fraction of ZnO or ZnS could be determined quantitatively in the range of 5-95% in the case of both powders and tablets. In analysis of the SA-BA systems, the weight fraction of SA or BA could be determined quantitatively in the range of 20-80% in the case of both powders and tablets. Quantitative analysis applying this pattern-fitting procedure showed better reproducibility than other X-ray methods based on the linear or integral intensities of particular diffraction peaks. Analysis using this pattern-fitting procedure also has the advantage that the preferred orientation of the crystallites in solid dosage forms can be also determined in the course of quantitative analysis.

Low cost synthesis of TiO2-C nanocomposite powder for high efficiency visible light photocatalysis

NASA Astrophysics Data System (ADS)

Mohapatra, A. K.; Nayak, J.

2018-04-01

Titanium dioxide-carbon nanocomposite powder was synthesized via a low cost chemical route using oleic acid and titanium tetra-isopropoxide. Since the carbon remained mainly on the surface of the TiO2 nanoparticles, the powder had black color. The composition of the powder was analyzed by X-ray photoelectron spectroscopy and the structure was studied with X-ray diffraction and transmission electron microscopy. The visible photocatalytic activity of the black TiO2 powder was investigated by studying the photo-bleaching of methylene blue under visible light. Our experimental observation showed that the black-TiO2 powder had a higher visible photocatalytic activity compared to the commercial TiO2 powder (P25 Degussa).

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

PubMed Central

2013-01-01

We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1H and 13C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1H and 13C chemical shifts for directly bonded 13C–1H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure. PMID:24386493

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids.

PubMed

Dudenko, Dmytro V; Williams, P Andrew; Hughes, Colan E; Antzutkin, Oleg N; Velaga, Sitaram P; Brown, Steven P; Harris, Kenneth D M

2013-06-13

We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1 H and 13 C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1 H and 13 C chemical shifts for directly bonded 13 C- 1 H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure.

Quantitative phase analysis of challenging samples using neutron powder diffraction. Sample #4 from the CPD QPA round robin revisited

DOE PAGES

Whitfield, Pamela S.

2016-04-29

Here, quantitative phase analysis (QPA) using neutron powder diffraction more often than not involves non-ambient studies where no sample preparation is possible. The larger samples and penetration of neutrons versus X-rays makes neutron diffraction less susceptible to inhomogeneity and large grain sizes, but most well-characterized QPA standard samples do not have these characteristics. Sample #4 from the International Union of Crystallography Commission on Powder Diffraction QPA round robin was one such sample. Data were collected using the POWGEN time-of-flight (TOF) neutron powder diffractometer and analysed together with historical data from the C2 diffractometer at Chalk River. The presence of magneticmore » reflections from Fe 3O 4 (magnetite) in the sample was an additional consideration, and given the frequency at which iron-containing and other magnetic compounds are present during in-operando studies their possible impact on the accuracy of QPA is of interest. Additionally, scattering from thermal diffuse scattering in the high-Qregion (<0.6 Å) accessible with TOF data could impact QPA results during least-squares because of the extreme peak overlaps present in this region. Refinement of POWGEN data was largely insensitive to the modification of longer d-spacing reflections by magnetic contributions, but the constant-wavelength data were adversely impacted if the magnetic structure was not included. A robust refinement weighting was found to be effective in reducing quantification errors using the constant-wavelength neutron data both where intensities from magnetic reflections were ignored and included. Results from the TOF data were very sensitive to inadequate modelling of the high- Q (low d-spacing) background using simple polynomials.« less

Iron oxide nanoparticles supported on ultradispersed diamond powders: Effect of the preparation procedure

NASA Astrophysics Data System (ADS)

Dimitrov, Momtchil; Ivanova, Ljubomira; Paneva, Daniela; Tsoncheva, Tanya; Stavrev, Stavry; Mitov, Ivan; Minchev, Christo

2009-01-01

The state of the iron oxide nanoparticles, supported on ultradispersed diamond (UDD) powders is studied by X-ray diffraction, nitrogen physisorption, temperature-programmed reduction, FTIR and Mössbauer spectroscopy. Methanol decomposition to hydrogen and CO is used as a catalytic test. The peculiarities of the iron oxide species strongly depend on the detonation procedure used for the UDD powders preparation as well as on the iron modification procedure.

Synthesis and characterization of titanium dioxide (TiO2) nanopowder

NASA Astrophysics Data System (ADS)

Munirah, S.; Nadzirah, Sh.; Khusaimi, Z.; Fazlena, H.; Rusop, M.

2018-05-01

Titanium dioxide (TiO2) powder was synthesized via sol-gel technique using Titanium tetraisopropoxide (TTIP) and ethanol as precursors. Acetylacetone, distilled water, polyethylene glycol (PEG) and stabilizers (glacial acetic acid and nitric acid) were then added to the solution. The solution was left for ageing for 24 hours and then dried into powder. The synthesized powders were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Thermogravimetric Analysis (TGA).

Spectroscopic detection of exogenous materials in latent fingerprints treated with powders and lifted off with adhesive tapes.

PubMed

Banas, A; Banas, K; Breese, M B H; Loke, J; Lim, S K

2014-07-01

Fingerprint evidence offers great value to criminal investigations since it is an internationally recognized and established means of human identification. With recent advances in modern technology, scientists have started analyzing not only the ridge patterns of fingerprints but also substances which can be found within them. The aim of this work was to determine whether Fourier transform infrared (FTIR) spectromicroscopy could be used to detect contamination in a fingerprint which was dusted with powder (a technique already recognized as an effective and reliable method for developing latent fingerprints) and subsequently lifted off with adhesive tape. Explosive materials (pentaerythritol tetranitrate, C-4, TNT) and noncontrolled substances (sugar, aspirin) were used to prepare contaminated fingerprints on various substrates. Freshly deposited fingermarks with powders which were lifted off with adhesive tapes (provided by Singapore Police Force) were analyzed using a Bruker Hyperion 2000 microscope at the ISMI beamline (Singapore Synchrotron Light Source) with an attenuated total reflection objective. FTIR spectroscopy is a nondestructive technique which requires almost no sample preparation. Further, the fingerprint under analysis remains in pristine condition, allowing subsequent analysis if necessary. All analyzed substances were successfully distinguished using their FTIR spectra in powdered and lifted fingerprints. This method has the potential to significantly impact forensic science by greatly enhancing the information that can be obtained from the study of fingerprints.

Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

NASA Astrophysics Data System (ADS)

Post, J. E.; Bish, D. L.; Heaney, P. J.

2006-05-01

Sepiolite is a hydrous Mg-silicate clay mineral with fibrous morphology that typically occurs as fine-grained, poorly crystalline masses. It occurs in a wide variety of geological environments and has been mined for centuries because of its many uses, e.g. in the pharmaceutical, fertilizer, and pesticide industries. Its versatile functionality derives from the large surface area and microporosity that are characteristic of the material. In recent years, sepiolite has received considerable attention with regard to the adsorption of organics, for use as a support for catalysts, as a molecular sieve, and as an inorganic membrane for ultrafiltration. Because of its fine-grained and poorly crystalline nature, it has not been possible to study sepiolite's crystal structure using single-crystal X-ray diffraction methods, and consequently many details of the structure are still not well known. In this study, Rietveld refinements using synchrotron powder X-ray diffraction data were used to investigate the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room- temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic water site. The RT structure under vacuum retained only ~1/8 of the zeolitic water and the volume decreased 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic water is lost by ~390 K, accompanied by a decrease in the a and c unit-cell parameters. Above ~600 K the sepiolite structure folds as one-half of the crystallographically bound water is lost. Rietveld refinements of the "anhydrous" sepiolite structure reveal that, in general, unit-cell parameters a, b, â and volume steadily decrease with increasing temperature; there is an obvious change in slope at ~820 K suggesting a phase transformation coinciding with the loss of the remaining bound water molecule. These temperature-resolved real-time powder X-ray diffraction studies provide the first comprehensive description of the sepiolite structure and the complex changes it undergoes as it dehydrates. Additional heating and cooling in situ powder X-ray diffraction experiments are underway in order to investigate the relative stabilities and rehydration behaviors of the partially-hydrated sepiolite phases. The results of these studies should provide a more robust model for predicting and modifying the properties and applications of this critical industrial material and environmentally important mineral.

An acoustic on-chip goniometer for room temperature macromolecular crystallography.

PubMed

Burton, C G; Axford, D; Edwards, A M J; Gildea, R J; Morris, R H; Newton, M I; Orville, A M; Prince, M; Topham, P D; Docker, P T

2017-12-05

This paper describes the design, development and successful use of an on-chip goniometer for room-temperature macromolecular crystallography via acoustically induced rotations. We present for the first time a low cost, rate-tunable, acoustic actuator for gradual in-fluid sample reorientation about varying axes and its utilisation for protein structure determination on a synchrotron beamline. The device enables the efficient collection of diffraction data via a rotation method from a sample within a surface confined droplet. This method facilitates efficient macromolecular structural data acquisition in fluid environments for dynamical studies.

1D silicon refractive lenses for surface scattering with high energy x-rays

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

Bertram, F.; Gutowski, O.; Schroer, C.

2016-07-27

At the high energy X-ray beamline P07 at PETRA III, 1D focusing down to 4 micrometer vertical beam height while preserving a horizontal beam width of 0.5 mm was established by refractive lenses etched into a silicon wafer. A single wafer with 8 different lens structures can cover the full energy range between 50 and 120 keV. For surface diffraction on ultrathin films a factor of 4 in intensity can be achieved compared to the already established Al-compound refractive 2D-lenses.

Focus of a multilayer Laue lens with an aperture of 102 microns determined by ptychography at beamline 1-BM at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Macrander, Albert; Wojcik, Michael; Maser, Jörg; Bouet, Nathalie; Conley, Raymond

2017-09-01

Ptychography was used to determine the focus of a Multilayer-Laue-Lens (MLL) at beamline 1-BM at the Advanced Photon Source (APS). The MLL had a record aperture of 102 microns with 15170 layers. The measurements were made at 12 keV. The focal length was 9.6 mm, and the outer-most zone was 4 nm thick. MLLs with ever larger apertures are under continuous development since ever longer focal lengths, ever larger working distances, and ever increased flux in the focus are desired. A focus size of 25 nm was determined by ptychographic phase retrieval from a gold grating sample with 1 micron lines and spaces over 3.0 microns horizontal distance. The MLL was set to focus in the horizontal plane of the bending magnet beamline. A CCD with 13.0 micron pixel size positioned 1.13 m downstream of the sample was used to collect the transmitted intensity distribution. The beam incident on the MLL covered the whole 102 micron aperture in the horizontal focusing direction and 20 microns in the vertical direction. 160 iterations of the difference map algorithm were sufficient to obtain a reconstructed image of the sample. The present work highlights the utility of a bending magnet source at the APS for performing coherence-based experiments. Use of ptychography at 1-BM on MLL optics opens the way to study diffraction-limited imaging of other hard x-ray optics.

Indium doped ZnO nano-powders prepared by RF thermal plasma treatment of In2O3 and ZnO

NASA Astrophysics Data System (ADS)

Lee, Mi-Yeon; Song, Min-Kyung; Seo, Jun-Ho; Kim, Min-Ho

2015-06-01

Indium doped ZnO nano-powders were synthesized by the RF thermal plasma treatment of In2O3 and ZnO. For this purpose, micron-sized ZnO powder was mixed with In2O3 powder at the In/Zn ratios of 0.0, 1.2, and 2.4 at. % by ball milling for 1 h, after which the mixtures were injected into RF thermal plasma generated at the plate power level of ˜140 kV A. As observed from the field emission scanning electron microscopy (FE-SEM) images of the RF plasma-treated powders, hexagonal prism-shaped nano-crystals were mainly obtained along with multi-pod type nano-particles, where the number of multi-pods decreased with increasing In/Zn ratios. In addition, the X-ray diffraction (XRD) data for the as-treated nano-powders showed the diffraction peaks for the In2O3 present in the precursor mixture to disappear, while the crystalline peaks for the single phase of ZnO structure shifted toward lower Bragg angles. In the UV-vis absorption spectra of the as-treated powders, redshifts were also observed with increases of the In/Zn ratios. Together with the FE-SEM images and the XRD data, the redshifts were indicative of the doping process of ZnO with indium, which took place during the RF thermal plasma treatment of In2O3 and ZnO.

Synchrotron X-ray CT characterization of titanium parts fabricated by additive manufacturing. Part I. Morphology.

PubMed

Scarlett, Nicola Vivienne Yorke; Tyson, Peter; Fraser, Darren; Mayo, Sheridan; Maksimenko, Anton

2016-07-01

Synchrotron X-ray tomography has been applied to the study of titanium parts fabricated by additive manufacturing (AM). The AM method employed here was the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V), as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron. Samples were chosen to examine the effect of build direction and complexity of design on the surface morphology and final dimensions of the piece.

Crystallization and Preliminary X-ray Diffraction Analysis of Hemextin A: A Unique Anticoagulant Protein from Hemachatus haemachatus Venom

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

Banerjee,Y.; Kumar, S.; Jobichen, C.

2007-01-01

Hemextin A was isolated and purified from African Ringhals cobra (Hemachatus haemachatus). It is a three-finger toxin that specifically inhibits blood coagulation factor VIIa and clot formation and that also interacts with hemextin B to form a unique anticoagulant complex. Hemextin A was crystallized by the hanging-drop vapor-diffusion method by equilibration against 0.2 M ammonium acetate, 0.1 M sodium acetate trihydrate pH 4.6 and 30% PEG 4000 as the precipitating agent. The crystals belong to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 49.27, b = 49.51, c = 57.87 {angstrom} and two molecules in the asymmetricmore » unit. They diffracted to 1.5 {angstrom} resolution at beamline X25 at BNL.« less

New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

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

Meng, Yue; Hrubiak, Rostislav; Rod, Eric

An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. Furthermore, the new capabilities have demonstrated clear benefits and provide new opportunities in researchmore » areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

DOE PAGES

Meng, Yue; Hrubiak, Rostislav; Rod, Eric; ...

2015-07-17

An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. Furthermore, the new capabilities have demonstrated clear benefits and provide new opportunities in researchmore » areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

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

Meng, Yue; Hrubiak, Rostislav; Rod, Eric

An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. The new capabilities have demonstrated clear benefits and provide new opportunities in research areasmore » including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

Micro structrual characterization and analysis of ball milled silicon carbide

NASA Astrophysics Data System (ADS)

Madhusudan, B. M.; Raju, H. P.; Ghanaraja., S.

2018-04-01

Mechanical alloying has been one of the prominent methods of powder synthesis technique in solid state involving cyclic deformation, cold welding and fracturing of powder particles. Powder particles in this method are subjected to greater mechanical deformation due to the impact of ball-powder-ball and ball-powder-container collisions that occurs during mechanical alloying. Strain hardening and fracture of particles decreases the size of the particles and creates new surfaces. The objective of this Present work is to use ball milling of SiC powder for different duration of 5, 10, 15 and 20 hours by High energy planetary ball milling machine and to evaluate the effect of ball milling on SiC powder. Micro structural Studies using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and EDAX has been investigated.

Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis.

PubMed

Moorhouse, Saul J; Wu, Yue; Buckley, Hannah C; O'Hare, Dermot

2016-11-24

We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses. During the flux synthesis of the n = 4 Aurivillius phase, Bi 5 Ti 3 Fe 0.5 Cr 0.5 O 15 at 950 °C in molten Na 2 SO 4 we observe the progression of numerous metastable phases. Using sequential multiphase Rietveld refinement of the time-dependent in situ XRD data, we are able to obtain mechanistic understanding of this reaction under a range of conditions.

Magnetic structure of Ho0.5Y0.5Mn6Sn6 compound studied by powder neutron diffraction

NASA Astrophysics Data System (ADS)

Li, X.-Y.; Peng, L.-C.; He, L.-H.; Zhang, S.-Y.; Yao, J.-L.; Zhang, Y.; Wang, F.-W.

2018-05-01

The crystallographic and magnetic structures of the HfFe6Ge6-type compound Ho0.5Y0.5Mn6Sn6 have been studied by powder neutron diffraction and in-situ Lorentz transmission electron microscopy. Besides the nonlinear thermal expansion of lattice parameters, an incommensurate conical spiral magnetic structure was determined in the temperature interval of 2-340 K. A spin reorientation transition has been observed from 50 to 300 K, where the alignment of the c-axis component of magnetic moments of the Ho sublattice and the Mn sublattice transfers from ferrimagnetic to ferromagnetic.

Crystal structure of pentasodium hydrogen dicitrate from synchrotron X-ray powder diffraction data and DFT comparison

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

Rammohan, Alagappa; Kaduk, James A.

2017-01-27

The crystal structure of pentasodium hydrogen dicitrate, Na 5H(C 6H 5O 7) 2, has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Each of the two independent citrate anions is joined into a dimer by very strong centrosymmetric O—H...O hydrogen bonds, with O...O distances of 2.419 and 2.409 Å. Four octahedrally coordinated Na +ions share edges to form open layers parallel to theabplane. A fifth Na +ion in trigonal–bipyramidal coordination shares faces with NaO 6octahedra on both sides of these layers.

In situ neutron diffraction study of micromechanical interactions and phase transformation in Ni-Mn-Ga alloy under uniaxial and hydrostatic stress.

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

Peng, R. L.; Wang, Y. D.; Nie, Z. H.

2008-01-01

This paper deals with the experimental study of stress-induced phase transformation in a polycrystalline Ni-Mn-Ga alloy under uniaxial compression and its powder under hydrostatic compression. In situ neutron diffraction experiments were employed to follow changes in the structure and lattice strains caused by the applied stresses. Large lattice strains that are dependent on the lattice planes or grain orientations were observed in the parent Heusler phase for both the bulk material and the powder sample. The development of such anisotropic strains and the influence of external load conditions are discussed in the paper.

High temperature phase stability in Li{sub 0.12}Na{sub 0.88}NbO{sub 3}: A combined powder X-ray and neutron diffraction study

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

Mishra, S. K.; Krishna, P. S. R.; Shinde, A. B.

2015-09-07

The phase stabilities of ecofriendly piezoelectric material of lithium doped sodium niobate for composition Li{sub 0.12}Na{sub 0.88}NbO{sub 3} (LNN12) have been investigated by a combination of powder X-ray and neutron diffraction techniques in the temperature range of 300–1100 K. We observed interesting changes with appearance or disappearance of the super-lattice reflections in the powder diffraction patterns. Unambiguous experimental evidence is shown for coexistence of paraelectric and ferroelectric orthorhombic phases in the temperature range of 525 K to 675 K. We identified the correct crystal structure of LNN12 with temperature and correlated it with observed anomaly in the physical properties. Identification of crystal structuremore » also helps in the mode assignments in Raman and infrared spectroscopies. We argued that application of chemical pressure as a result of Li substitution in NaNbO{sub 3} matrix favors the freezing of zone centre phonons in contrast to the freezing of zone boundary phonons in pure NaNbO{sub 3} with the variation of temperature.« less

Combined Approach for the Structural Characterization of Alkali Fluoroscandates: Solid-State NMR, Powder X-ray Diffraction, and Density Functional Theory Calculations.

PubMed

Rakhmatullin, Aydar; Polovov, Ilya B; Maltsev, Dmitry; Allix, Mathieu; Volkovich, Vladimir; Chukin, Andrey V; Boča, Miroslav; Bessada, Catherine

2018-02-05

The structures of several fluoroscandate compounds are presented here using a characterization approach combining powder X-ray diffraction and solid-state NMR. The structure of K 5 Sc 3 F 14 was fully determined from Rietveld refinement performed on powder X-ray diffraction data. Moreover, the local structures of NaScF 4 , Li 3 ScF 6 , KSc 2 F 7 , and Na 3 ScF 6 compounds were studied in detail from solid-state 19 F and 45 Sc NMR experiments. The 45 Sc chemical shift ranges for six- and seven-coordinated scandium environments were defined. The 19 F chemical shift ranges for bridging and terminal fluorine atoms were also determined. First-principles calculations of the 19 F and 45 Sc NMR parameters were carried out using plane-wave basis sets and periodic boundary conditions (CASTEP), and the results were compared with the experimental data. A good agreement between the calculated shielding constants and experimental chemical shifts was obtained. This demonstrates the good potential of computational methods in spectroscopic assignments of solid-state 45 Sc NMR spectroscopy.

Characterization of cubic ceria?zirconia powders by X-ray diffraction and vibrational and electronic spectroscopy

NASA Astrophysics Data System (ADS)

Sánchez Escribano, Vicente; Fernández López, Enrique; Panizza, Marta; Resini, Carlo; Gallardo Amores, José Manuel; Busca, Guido

2003-10-01

The X-ray diffraction (XRD) patterns and the Infrared, Raman and UV-visible spectra of CeO 2ZrO 2 powders prepared by co-precipitation are presented. Raman spectra provide evidence for the largely predominant cubic structure of the powders with CeO 2 molar composition higher than 25%. Also skeletal IR spectra allow to distinguish cubic from tetragonal phases which are instead not easily distinguished on the basis of the XRD patterns. All mixed oxides including pure ceria are strong UV absorbers although also absorb in the violet visible region. By carefully selecting their composition and treatment temperature, the onset of the radiation that they cut off can be chosen in the 425-475 nm interval. Although they are likely metastable, the cubic phases are still pure even after heating at 1173 K for 4 h.

Structural, mechanical, electrical and optical properties of a new lithium boro phthalate NLO crystal synthesized by a slow evaporation method

NASA Astrophysics Data System (ADS)

Mohanraj, K.; Balasubramanian, D.; Jhansi, N.

2017-11-01

A new non-linear optical (NLO) single crystal of lithium boro phthalate (LiBP) was grown by slow solvent evaporation technique. The powder sample was subjected to powder X-ray diffraction (PXRD) to find its crystalline nature and the crystal structure of the grown crystal was determined using single crystal X-ray (SXRD) diffraction analysis. The Fourier Transform Infrared (FTIR) spectrum was recorded for grown crystal to identify the various functional groups present in the compound. The mechanical property of the LiBP single crystal was studied using Vickers microhardness tester. The dielectric constant and dielectric loss measurements were carried out for the grown crystal at various temperatures. The grown crystal was subjected to UV-Visible Spectral Studies to analyze the linear optical behavior of the grown crystal. The Kurtz-Perry Powder technique was employed to measure the Second Harmonic Generation efficiency of the grown crystal.

POWTEX - A new High-Intensity Powder and Texture Diffractometer at FRM II, Garching Germany

NASA Astrophysics Data System (ADS)

Walter, J. M.; Brückel, T.; Dronskowski, R.; Hansen, B. T.; Houben, A.; Klein, H.; Leiss, B.; Vollbrecht, A.; Sowa, H.

2009-05-01

In recent years, neutron diffraction has become a routine tool in Geoscience for experimental high-field (HP/HT/HH) powder diffraction and for the quantitative analysis of the crystallographic preferred orientation (CPO). Quantitative texture analysis is e.g. involved in the research fields of fabric development in mono- and polyphase rocks, deformation histories and kinematics during mountain building processes and the characterization of flow kinematics in lava flows. Secondly the quantitative characterization of anisotropic physical properties of both rock and analogue materials is conducted by bulk texture measurements of sometimes larger sample volumes. This is easily achievable by neutron diffraction due to the high penetration capabilities of the neutrons. The resulting geoscientific need for increased measuring time at neutron diffraction facilities with the corresponding technical characteristics and equipment will in future be satisfied by this high-intensity diffractometer at the neutron research reactor FRM II in Garching, Germany. It will be built by a consortium of groups from the RWTH Aachen, Forschungszentrum Jülich and the University of Göttingen, who will also operate the instrument. The diffractometer will be optimized to high intensities (flux) with an equivalent sufficient resolution for polyphase rocks. Furthermore a broad range of d-values (0.5 to 15 Å) will be measurable. The uniqueness of this instrument is the geoscientific focus on different sample environments for in situ-static and deformation experiments (stress, strain and annealing/recrystallisation) and (U)HP/(U)HT experiments. A LP/LT or atmospheric-P deformation rig for in situ-deformation experiments on ice, halite or rock analogue materials is planned, to allow in situ-measurements of the texture development during deformation and annealing. Additionally a uniaxial HT/MP deformation apparatus for salt deformation experiments and an adapted Griggs- type deformation rig are also designated. Furthermore an uniaxial stress frame for in situ stress investigations is planned to conduct simultaneous measurements of stress, elastic or plastic deformation and texture. Other sample environments for geoscientific application will be HP/HT furnaces and pressure cells for powder diffraction investigations. Furthermore the diffractometer will be built in combination with a high-pressure multi anvil up to 25 GPa and 2500 K built by the University of Bayreuth at the same beam line. The detector concept allows single shot texture measurements and therefore the measurement of larger geological sample series as necessary for the investigations of complete geological structures. This concept is complementary to the geoscience neutron texture diffractometer in Dubna, Russia and the stress diffractometer STRESS-SPEC located also at the Garching research reactor. For powder diffraction the diffractometer will be complementary to the existing high-resolution powder diffractometer SPODI at the FRM-II. It will offer the possibility of short, high-intensity parametric powder diffraction measurements in dependency of temperature, electrical, magnetic and stress fields due to the higher flux at the sample. The optimization to high-intensities and therefore short measuring times will also allow time-resolved measurements of kinetic reactions even of small sample volumes.

Single-crystal diffraction at megabar conditions by synchrotron radiation

NASA Astrophysics Data System (ADS)

Merlini, Marco; Hanfland, Michael

2013-08-01

Crystal structure determination at extreme pressures is currently possible at synchrotron beamlines optimized for such a purpose. We report the description of the experimental setup available at European Synchrotron Radiation Facility ID09 beamline (Grenoble, France) and, with two examples, we illustrate the state-of-the-art experiments currently performed at third-generation synchrotrons. The first example concerns the determination of the equation of state and the structural behavior of low-spin Fe-bearing siderite in the megabar pressure range. Siderite, in fact, undergoes a first-order isosymmetric transition at 45 GPa, and, above this pressure, it features Fe2+ in electronic low-spin configuration. The local configuration of Fe coordination polyhedra, determined by structural refinements, significantly deviates from a regular octahedron. Nevertheless, no further structural transition is detected up to the maximum pressure reached in our experiments, 135 GPa. The analysis of the Fe-O bond length extrapolated to ambient pressure, which indicates that the difference in ionic radii between the high- and the low-spin state of Fe2+ is 0.172 Å, in excellent agreement with the tabulated data by Shannon and Prewitt [Effective ionic radii in oxides and fluorides. Acta Crystallogr. 1969;B25:925-946]. The second example concerns the determination and refinement of the oP8 structure adopted by sodium in the pressure interval 118-125 GPa, using an experimental dataset collected at 118 GPa. The orthorhombic [a=4.7687(15) Å, b=3.0150(6) Å, c=5.2423(7) Å, V=75.4(3) Å3] oP8 structure is topologically related to the MnP structure, with two non-equivalent atoms in the unit cell. Despite the weak scattering factor of Na atoms, the quality of the data also allows meaningful displacement parameters refinements (R1=4.6%, 14 parameters, 190 diffractions, and 105 unique) demonstrating that the current accuracy of diffraction data at extreme pressures can be comparable with ambient condition measurements.

Optical, Physical, and Chemical Properties of Surface Modified Titanium Dioxide Powders

DTIC Science & Technology

2011-02-01

coefficient depends on the optical efficiency factor, QCM , the geometric cross section, G, and the particle mass as indicated by the relationship in eq 2...diffraction sensor with a RODOS powder dispersing unit. The instrument houses a HeNe laser (632.8 nm) and Fourier lens. Upon introduction of the

Physicochemical characterization of tacrolimus-loaded solid dispersion with sodium carboxylmethyl cellulose and sodium lauryl sulfate.

PubMed

Park, Young-Joon; Ryu, Dong-Sung; Li, Dong Xun; Quan, Qi Zhe; Oh, Dong Hoon; Kim, Jong Oh; Seo, Youn Gee; Lee, Young-Im; Yong, Chul Soon; Woo, Jong Soo; Choi, Han-Gon

2009-06-01

To develop a novel tacrolimus-loaded solid dispersion with improved solubility, various solid dispersions were prepared with various ratios of water, sodium lauryl sulfate, citric acid and carboxylmethylcellulose-Na using spray drying technique. The physicochemical properties of solid dispersions were investigated using scanning electron microscopy, differential scanning calorimetery and powder X-ray diffraction. Furthermore, their solubility and dissolution were evaluated compared to drug powder. The solid dispersion at the tacrolimus/CMC-Na/sodium lauryl sulfate/citric acid ratio of 3/24/3/0.2 significantly improved the drug solubility and dissolution compared to powder. The scanning electron microscopy result suggested that carriers might be attached to the surface of drug in this solid dispersion. Unlike traditional solid dispersion systems, the crystal form of drug in this solid dispersion could not be converted to amorphous form, which was confirmed by the analysis of DSC and powder X-ray diffraction. Thus, the solid dispersion system with water, sodium lauryl sulfate, citric acid and CMC-Na should be a potential candidate for delivering a poorly water-soluble tacrolimus with enhanced solubility and no convertible crystalline.

Nano-Crystalline Thermally Evaporated Bi2Se3 Thin Films Synthesized from Mechanically Milled Powder

NASA Astrophysics Data System (ADS)

Amara, A.; Abdennouri, N.; Drici, A.; Abdelkader, D.; Bououdina, M.; Chaffar Akkari, F.; Khemiri, N.; Kanzari, M.; Bernède, J. C.

2017-08-01

Bi2Se3 powder has been successfully synthesized via mechanical ball milling of bismuth and selenium as starting materials. X-ray diffraction characterization revealed the formation of the rhombohedral and orthorhombic phases of Bi2Se3 material belonging to systems with space groups R\\bar{3}m and Pbnm, respectively. The advantageous last finding is confirmed by the Rietveld refinement of the x-ray diffraction data. Furthermore, the analysis of the x-ray data of thermally deposited thin films revealed that both orthorhombic and rhombohedral phases are coexisting in the layer. The morphology of the ball milled powder was studied by scanning electron microscopy. The phase formation of the material is confirmed by Raman spectroscopy. M-H (Magnetization versus Magnetic field) curve indicates that Bi2Se3 powder has a ferromagnetic behavior. Additionally, absorbance and transmittance measurements were carried out on the obtained thermally evaporated thin films and yielded a band gap of 1.33 eV supporting the potential application of the heterogeneous rhombohedral/orthorhombic Bi2Se3 material in photovoltaics.

Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

NASA Astrophysics Data System (ADS)

Lin, Chia-Hsuan; Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Moo-Chin; Ko, Horng-Huey

2017-12-01

The synthesis and optical properties of Mg-Al layered double hydroxide (LDH) precursor powders were investigated using X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution TEM (HRTEM), UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363-1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH)2](CO3)0.083.(H2O)0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL) spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

Effect of microfibril twisting in theoretical powder diffraction studies of cellulose Iß

USDA-ARS?s Scientific Manuscript database

Previous studies of calculated diffraction patterns for cellulose crystallites have suggested that the distortions arising once models have been subjected to MD simulation are likely the result of dimensional changes induced by the empirical force field, but have been unable to determine to what ext...

On the influence of monochromator thermal deformations on X-ray focusing

DOE PAGES

Antimonov, M. A.; Khounsary, A. M.; Sandy, A. R.; ...

2016-03-02

A cooled double crystal monochromator system is used on many high heat load X-ray synchrotron radiation beamlines in order to select, by diffraction, a narrow spectrum of the beam. Thermal deformation of the first crystal monochromator – and the potential loss of beam brightness – is often a concern. However, if downstream beam focusing is planned, the lensing effect of the monochromator must be considered even if thermal deformations are small. In this paper we report on recent experiments at an Advanced Photon Source (APS) beamline that focuses the X-ray beam using compound refractive lenses downstream of an X-ray monochromatormore » system. Increasing the X-ray beam power by increasing the storage ring current from 100 mA to 130 mA resulted in an effective doubling of the focal distance. We show quantitatively that this is due to a lensing effect of the distorted monochromator that results in the creation of a virtual source downstream of the actual source. Lastly, an analysis of the defocusing and options to mitigate this effect are explored.« less

Compensation of X-ray mirror shape-errors using refractive optics

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

Sawhney, Kawal, E-mail: Kawal.sawhney@diamond.ac.uk; Laundy, David; Pape, Ian

2016-08-01

Focusing of X-rays to nanometre scale focal spots requires high precision X-ray optics. For nano-focusing mirrors, height errors in the mirror surface retard or advance the X-ray wavefront and after propagation to the focal plane, this distortion of the wavefront causes blurring of the focus resulting in a limit on the spatial resolution. We describe here the implementation of a method for correcting the wavefront that is applied before a focusing mirror using custom-designed refracting structures which locally cancel out the wavefront distortion from the mirror. We demonstrate in measurements on a synchrotron radiation beamline a reduction in the sizemore » of the focal spot of a characterized test mirror by a factor of greater than 10 times. This technique could be used to correct existing synchrotron beamline focusing and nanofocusing optics providing a highly stable wavefront with low distortion for obtaining smaller focus sizes. This method could also correct multilayer or focusing crystal optics allowing larger numerical apertures to be used in order to reduce the diffraction limited focal spot size.« less

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

Meng, Xiangyu; Shi, Xianbo; Wang, Yong

The mutual optical intensity (MOI) model is extended to include the propagation of partially coherent radiation through non-ideal mirrors. The propagation of the MOI from the incident to the exit plane of the mirror is realised by local ray tracing. The effects of figure errors can be expressed as phase shifts obtained by either the phase projection approach or the direct path length method. Using the MOI model, the effects of figure errors are studied for diffraction-limited cases using elliptical cylinder mirrors. Figure errors with low spatial frequencies can vary the intensity distribution, redistribute the local coherence function and distortmore » the wavefront, but have no effect on the global degree of coherence. The MOI model is benchmarked againstHYBRIDand the multi-electronSynchrotron Radiation Workshop(SRW) code. The results show that the MOI model gives accurate results under different coherence conditions of the beam. Other than intensity profiles, the MOI model can also provide the wavefront and the local coherence function at any location along the beamline. The capability of tuning the trade-off between accuracy and efficiency makes the MOI model an ideal tool for beamline design and optimization.« less

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

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

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

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

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

PubMed Central

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

2015-01-01

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

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

DOE PAGES

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

2015-04-08

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

Oxidized nanocrystalline Fe-Cu pseudoalloy subjected to high pressure and electrodischarge pulses: Mössbauer and x-ray investigations

NASA Astrophysics Data System (ADS)

Gavriliuk, A. G.; Voitkovsky, V. S.; Sidorov, V. A.; Filonenko, V. P.; Tsiok, O. B.; Khvostantsev, L. G.

1998-05-01

Nanocrystalline Fe15Cu85 pseudoalloy has been subjected to pulsed heating up to 1500 K at high pressure (8 GPa). Two regimes were studied: the direct heating using electrodischarge through the sample and indirect heating with the use of cylindrical heater around the sample. The temperature and time conditions in both types of experiments were adjusted to be equivalent. The discharge parameters (stored energy, discharge time, and magnitude of current pulse) were sufficient to move defects by conduction electrons, but insufficient to melt the sample. The properties of treated samples were studied using Mössbauer absorption spectra and x-ray diffraction for three types of samples: (a) primary powder treated by high pressure up to 8 GPa, (b) powder subjected to indirect pulsed heating at 8 GPa, (c) powder treated by electrical pulses at 8 GPa. The x-ray diffraction pattern of primary powder exhibits peaks of copper, iron, and copper oxide (CuO). The Mössbauer spectrum of primary powder exhibits six peaks of alpha iron and some peaks near zero velocity due to the small iron clusters in the copper matrix and ultrafine clusters of paramagnetic phase x-Fe2O3. The transformation of CuO to Cu2O takes place in the course of indirect heating, the Mössbauer spectrum being almost unchanged. The direct electrodischarge heating causes the appearance of new magnetic phase with the magnetic field on iron nucleus 505 kOe, which corresponds to α-Fe2O3. The formation of α-Fe2O3 was confirmed by x-ray diffraction. At the same time the transformation of CuO to Cu2O is incomplete. These experiments demonstrate that high density current pulses, causing the electron wind, can be a useful tool to influence the structure of nanocrystalline powder.

Preparation and antibacterial properties of titanium-doped ZnO from different zinc salts

PubMed Central

2014-01-01

To research the relationship of micro-structures and antibacterial properties of the titanium-doped ZnO powders and probe their antibacterial mechanism, titanium-doped ZnO powders with different shapes and sizes were prepared from different zinc salts by alcohothermal method. The ZnO powders were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy (UV-vis), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED), and the antibacterial activities of titanium-doped ZnO powders on Escherichia coli and Staphylococcus aureus were evaluated. Furthermore, the tested strains were characterized by SEM, and the electrical conductance variation trend of the bacterial suspension was characterized. The results indicate that the morphologies of the powders are different due to preparation from different zinc salts. The XRD results manifest that the samples synthesized from zinc acetate, zinc nitrate, and zinc chloride are zincite ZnO, and the sample synthesized from zinc sulfate is the mixture of ZnO, ZnTiO3, and ZnSO4 · 3Zn (OH)2 crystal. UV-vis spectra show that the absorption edges of the titanium-doped ZnO powders are red shifted to more than 400 nm which are prepared from zinc acetate, zinc nitrate, and zinc chloride. The antibacterial activity of titanium-doped ZnO powders synthesized from zinc chloride is optimal, and its minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) are lower than 0.25 g L−1. Likewise, when the bacteria are treated by ZnO powders synthesized from zinc chloride, the bacterial cells are damaged most seriously, and the electrical conductance increment of bacterial suspension is slightly high. It can be inferred that the antibacterial properties of the titanium-doped ZnO powders are relevant to the microstructure, particle size, and the crystal. The powders can damage the cell walls; thus, the electrolyte is leaked from cells. PMID:24572014

L-Leucine as an excipient against moisture on in vitro aerosolization performances of highly hygroscopic spray-dried powders.

PubMed

Li, Liang; Sun, Siping; Parumasivam, Thaigarajan; Denman, John A; Gengenbach, Thomas; Tang, Patricia; Mao, Shirui; Chan, Hak-Kim

2016-05-01

L-Leucine (LL) has been widely used to enhance the dispersion performance of powders for inhalation. LL can also protect powders against moisture, but this effect is much less studied. The aim of this study was to investigate whether LL could prevent moisture-induced deterioration in in vitro aerosolization performances of highly hygroscopic spray-dried powders. Disodium cromoglycate (DSCG) was chosen as a model drug and different amounts of LL (2-40% w/w) were added to the formulation, with the aim to explore the relationship between powder dispersion, moisture protection and physicochemical properties of the powders. The powder formulations were prepared by spray drying of aqueous solutions containing known concentrations of DSCG and LL. The particle sizes were measured by laser diffraction. The physicochemical properties of fine particles were characterized by X-ray powder diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and dynamic vapor sorption (DVS). The surface morphology and chemistry of fine particles were analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (ToF-SIMS). In vitro aerosolization performances were evaluated by a next generation impactor (NGI) after the powders were stored at 60% or 75% relative humidity (RH), and 25°C for 24h. Spray-dried (SD) DSCG powders were amorphous and absorbed 30-45% (w/w) water at 70-80% RH, resulting in deterioration in the aerosolization performance of the powders. LL did not decrease the water uptake of DSCG powders, but it could significantly reduce the effect of moisture on aerosolization performances. This is due to enrichment of crystalline LL on the surface of the composite particles. The effect was directly related to the percentage of LL coverage on the surface of particles. Formulations having 61-73% (molar percent) of LL on the particle surface (which correspond to 10-20% (w/w) of LL in the bulk powders) could minimize moisture-induced deterioration in the aerosol performance. In conclusion, particle surface coverage of LL can offer short-term protection against moisture on dispersion of hygroscopic powders. Copyright © 2016 Elsevier B.V. All rights reserved.

One-Step Hydrothermal-Electrochemical Route to Carbon-Stabilized Anatase Powders

NASA Astrophysics Data System (ADS)

Tao, Ying; Yi, Danqing; Zhu, Baojun

2013-04-01

Black carbon-stabilized anatase particles were prepared by a simple one-step hydrothermal-electrochemical method using glucose and titanium citrate as the carbon and titanium source, respectively. Morphological, chemical, structural, and electrochemical characterizations of these powders were carried out by Raman spectroscopy, Fourier-transform infrared spectroscopy, x-ray diffraction, scanning electron microscopy, and cyclic voltammetry. It was revealed that 200-nm carbon/anatase TiO2 was homogeneously dispersed, and the powders exhibited excellent cyclic performance at high current rates of 0.05 V/s. The powders are interesting potential materials that could be used as anodes for lithium-ion batteries.

Probing hydrogen positions in hydrous compounds: information from parametric neutron powder diffraction studies.

PubMed

Ting, Valeska P; Henry, Paul F; Schmidtmann, Marc; Wilson, Chick C; Weller, Mark T

2012-05-21

We demonstrate the extent to which modern detector technology, coupled with a high flux constant wavelength neutron source, can be used to obtain high quality diffraction data from short data collections, allowing the refinement of the full structures (including hydrogen positions) of hydrous compounds from in situ neutron powder diffraction measurements. The in situ thermodiffractometry and controlled humidity studies reported here reveal that important information on the reorientations of structural water molecules with changing conditions can be easily extracted, providing insight into the effects of hydrogen bonding on bulk physical properties. Using crystalline BaCl2·2H2O as an example system, we analyse the structural changes in the compound and its dehydration intermediates with changing temperature and humidity levels to demonstrate the quality of the dynamic structural information on the hydrogen atoms and associated hydrogen bonding that can be obtained without resorting to sample deuteration.

Structure investigations of ferromagnetic Co-Ni-Al alloys obtained by powder metallurgy.

PubMed

Maziarz, W; Dutkiewicz, J; Lityńska-Dobrzyńska, L; Santamarta, R; Cesari, E

2010-03-01

Elemental powders of Co, Ni and Al in the proper amounts to obtain Co(35)Ni(40)Al(25) and Co(40)Ni(35)Al(25) nominal compositions were ball milled in a high-energy mill for 80 h. After 40 h of milling, the formation of a Co (Ni, Al) solid solution with f.c.c. structure was verified by a change of the original lattice parameter and crystallite size. Analytical transmission electron microscopy observations and X-ray diffraction measurements of the final Co (Ni, Al) solid solution showed that the crystallite size scattered from 4 to 8 nm and lattice parameter a = 0.36086 nm. The chemical EDS point analysis of the milled powder particles allowed the calculation of the e/a ratio and revealed a high degree of chemical homogeneity of the powders. Hot pressing in vacuum of the milled powders resulted in obtaining compacts with a density of about 70% of the theoretical one. An additional heat treatment increased the density and induced the martensitic transformation in a parent phase. Selected area diffraction patterns and dark field images obtained from the heat-treated sample revealed small grains around 300 nm in diameter consisting mainly of the ordered gamma phase (gamma'), often appearing as twins, and a small amount of the L1(0) ordered martensite.

Design and physicochemical characterization of advanced spray-dried tacrolimus multifunctional particles for inhalation

PubMed Central

Wu, Xiao; Hayes, Don; Zwischenberger, Joseph B; Kuhn, Robert J; Mansour, Heidi M

2013-01-01

The aim of this study was to design, develop, and optimize respirable tacrolimus microparticles and nanoparticles and multifunctional tacrolimus lung surfactant mimic particles for targeted dry powder inhalation delivery as a pulmonary nanomedicine. Particles were rationally designed and produced at different pump rates by advanced spray-drying particle engineering design from organic solution in closed mode. In addition, multifunctional tacrolimus lung surfactant mimic dry powder particles were prepared by co-dissolving tacrolimus and lung surfactant mimic phospholipids in methanol, followed by advanced co-spray-drying particle engineering design technology in closed mode. The lung surfactant mimic phospholipids were 1,2-dipalmitoyl-sn-glycero-3-phosphocholine and 1,2-dipalmitoyl-sn-glycero-3-[phosphor-rac-1-glycerol]. Laser diffraction particle sizing indicated that the particle size distributions were suitable for pulmonary delivery, whereas scanning electron microscopy imaging indicated that these particles had both optimal particle morphology and surface morphology. Increasing the pump rate percent of tacrolimus solution resulted in a larger particle size. X-ray powder diffraction patterns and differential scanning calorimetry thermograms indicated that spray drying produced particles with higher amounts of amorphous phase. X-ray powder diffraction and differential scanning calorimetry also confirmed the preservation of the phospholipid bilayer structure in the solid state for all engineered respirable particles. Furthermore, it was observed in hot-stage micrographs that raw tacrolimus displayed a liquid crystal transition following the main phase transition, which is consistent with its interfacial properties. Water vapor uptake and lyotropic phase transitions in the solid state at varying levels of relative humidity were determined by gravimetric vapor sorption technique. Water content in the various powders was very low and well within the levels necessary for dry powder inhalation, as quantified by Karl Fisher coulometric titration. Conclusively, advanced spray-drying particle engineering design from organic solution in closed mode was successfully used to design and optimize solid-state particles in the respirable size range necessary for targeted pulmonary delivery, particularly for the deep lung. These particles were dry, stable, and had optimal properties for dry powder inhalation as a novel pulmonary nanomedicine. PMID:23403805

Influence of grinding on service properties of VT-22 powder applied in additive technologies

NASA Astrophysics Data System (ADS)

Zakharov, M. N.; Rybalko, O. F.; Romanova, O. V.; Gelchinskiy, B. R.; Il'inykh, S. A.; Krashaninin, V. A.

2017-01-01

Powder of titanium alloy (VT-22) produced by plasma-spraying was subjected to grinding to obtain powder with size less 100 microns. These powders were sprayed by plasma unit using two types of gases, namely, air and air with methane (spraying in water and sputtering of coating on steel support). Influence of grinding time on yield of powder of required fraction was studied. Morphology and phase composition of the grinded powder and plasma sprayed one were under investigation. In the result of experiments, it appears that the grinding time genuinely influences the chemical and phase compositions, but there is no effect on physical-processing properties. For powders after plasma spraying some changes of non-metal elements content were detected by chemical analysis. Using gaseous mixture of air and methane in plasma spraying unit leads to formation of a new phase in the powder according X-ray diffraction data.

Compact, Non-Pneumatic Rock-Powder Samplers

NASA Technical Reports Server (NTRS)

Sherrit, Stewart; Bar-Cohen, Yoseph; Badescu, Mircea; Bao, Xiaoqi; Chang, Zensheu; Jones, Christopher; Aldrich, Jack

2008-01-01

Tool bits that automatically collect powdered rock, permafrost, or other hard material generated in repeated hammering action have been invented. The present invention pertains to the special case in which it is desired to collect samples in powder form for analysis by x-ray diffraction and possibly other techniques. The present invention eliminates the need for both the mechanical collection equipment and the crushing chamber and the pneumatic collection equipment of prior approaches, so that it becomes possible to make the overall sample-acquisition apparatus more compact.

Time-resolved in situ neutron diffraction under supercritical hydrothermal conditions: a study of the synthesis of KTiOPO4.

PubMed

Ok, Kang Min; Lee, Dong Woo; Smith, Ronald I; O'Hare, Dermot

2012-10-31

In the first in situ neutron powder diffraction study of a supercritical hydrothermal synthesis, the crystallization of KTiOPO(4) (KTP) at 450 °C and 380 bar has been investigated. The time-resolved diffraction data suggest that the crystallization of KTP occurs by the reaction between dissolved K(+)(aq), PO(4)(3-)(aq), and [Ti(OH)(x)]((4-x)+)(aq) species.

Experimental measurement of lattice strain pole figures using synchrotron x rays

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

Miller, M.P.; Bernier, J.V.; Park, J.-S.

This article describes a system for mechanically loading test specimens in situ for the determination of lattice strain pole figures and their evolution in multiphase alloys via powder diffraction. The data from these experiments provide insight into the three-dimensional mechanical response of a polycrystalline aggregate and represent an extremely powerful material model validation tool. Relatively thin (0.5 mm) iron/copper specimens were axially strained using a mechanical loading frame beyond the macroscopic yield strength of the material. The loading was halted at multiple points during the deformation to conduct a diffraction experiment using a 0.5x0.5 mm{sup 2} monochromatic (50 keV) xmore » ray beam. Entire Debye rings of data were collected for multiple lattice planes ({l_brace}hkl{r_brace}'s) in both copper and iron using an online image plate detector. Strain pole figures were constructed by rotating the loading frame about the specimen transverse direction. Ideal powder patterns were superimposed on each image for the purpose of geometric correction. The chosen reference material was cerium (IV) oxide powder, which was spread in a thin layer on the downstream face of the specimen using petroleum jelly to prevent any mechanical coupling. Implementation of the system at the A2 experimental station at the Cornell High Energy Synchrotron Source (CHESS) is described. The diffraction moduli measured at CHESS were shown to compare favorably to in situ data from neutron-diffraction experiments conducted on the same alloys.« less

Sealed-tube synthesis and phase diagram of Li{sub x}TiS{sub 2} (0 ≤ x ≤1)

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

Zhang, Ziping; National Laboratory for Superconductivity, Institute of Physics, Chinese Academy of Science, Beijing 100190; Dong, Cheng, E-mail: chengdon@aphy.iphy.ac.cn

2015-01-15

Graphical abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S aslithium source. A schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed based on the DTA and XRD data. - Abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S as lithium source. The Li{sub x}TiS{sub 2} samples were characterized by powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and differential thermal analysis. Themore » variations of the lattice parameters with lithium content x in Li{sub x}TiS{sub 2} were determined by X-ray powder diffraction analysis for both 1T and 3R phases. The phase transition between low-temperature 1T phase and high-temperature 3R phase was confirmed by the powder X-ray diffraction analysis. Based on the differential thermal analysis and X-ray diffraction results, a schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed, providing a guideline to synthesize Li{sub x}TiS{sub 2} in 1T structure or 3R structure.« less

Characterization of the carbides and the martensite phase in powder-metallurgy high-speed steel

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

Godec, Matjaz, E-mail: matjaz.godec@imt.si; Batic, Barbara Setina; Mandrino, Djordje

2010-04-15

A microstructural characterization of the powder-metallurgy high-speed-steel S390 Microclean was performed based on an elemental distribution of the carbide phase as well as crystallographic analyses. The results showed that there were two types of carbides present: vanadium-rich carbides, which were not chemically homogeneous and exhibited a tungsten-enriched or tungsten-depleted central area; and chemically homogeneous tungsten-rich M{sub 6}C-type carbides. Despite the possibility of chemical inhomogenities, the crystallographic orientation of each of the carbides was shown to be uniform. Using electron backscatter diffraction the vanadium-rich carbides were determined to be either cubic VC or hexagonal V{sub 6}C{sub 5}, while the tungsten-rich carbidesmore » were M{sub 6}C. The electron backscatter diffraction results were also verified using X-ray diffraction. Several electron backscatter diffraction pattern maps were acquired in order to define the fraction of each carbide phase as well as the amount of martensite phase. The fraction of martensite was estimated using band-contrast images, while the fraction of carbides was calculated using the crystallographic data.« less

A wavelet transform algorithm for peak detection and application to powder x-ray diffraction data.

PubMed

Gregoire, John M; Dale, Darren; van Dover, R Bruce

2011-01-01

Peak detection is ubiquitous in the analysis of spectral data. While many noise-filtering algorithms and peak identification algorithms have been developed, recent work [P. Du, W. Kibbe, and S. Lin, Bioinformatics 22, 2059 (2006); A. Wee, D. Grayden, Y. Zhu, K. Petkovic-Duran, and D. Smith, Electrophoresis 29, 4215 (2008)] has demonstrated that both of these tasks are efficiently performed through analysis of the wavelet transform of the data. In this paper, we present a wavelet-based peak detection algorithm with user-defined parameters that can be readily applied to the application of any spectral data. Particular attention is given to the algorithm's resolution of overlapping peaks. The algorithm is implemented for the analysis of powder diffraction data, and successful detection of Bragg peaks is demonstrated for both low signal-to-noise data from theta-theta diffraction of nanoparticles and combinatorial x-ray diffraction data from a composition spread thin film. These datasets have different types of background signals which are effectively removed in the wavelet-based method, and the results demonstrate that the algorithm provides a robust method for automated peak detection.

Synthesis of TiCx Powder via the Underwater Explosion of an Explosive

NASA Astrophysics Data System (ADS)

Tanaka, Shigeru; Bataev, Ivan; Hamashima, Hideki; Tsurui, Akihiko; Hokamoto, Kazuyuki

2018-05-01

In this study, a novel approach to the explosive synthesis of titanium carbide (TiC) is discussed. Nonstoichiometric TiCx powder was produced via the underwater explosion of a Ti powder encapsulated within a spherical explosive charge. The explosion process, bubble formation, and synthesis process were visualized using high-speed camera imaging. It was concluded that synthesis occurred within the detonation gas during the first expansion/contraction cycle of the bubble, which was accompanied by a strong emission of light. The recovered powders were studied using scanning electron microscopy and X-ray diffraction. Submicron particles were generated during the explosion. An increase in the carbon content of the starting powder resulted in an increase in the carbon content of the final product. No oxide byproducts were observed within the recovered powders.

Powder X-ray diffraction laboratory, Reston, Virginia

USGS Publications Warehouse

Piatak, Nadine M.; Dulong, Frank T.; Jackson, John C.; Folger, Helen W.

2014-01-01

The powder x-ray diffraction (XRD) laboratory is managed jointly by the Eastern Mineral and Environmental Resources and Eastern Energy Resources Science Centers. Laboratory scientists collaborate on a wide variety of research problems involving other U.S. Geological Survey (USGS) science centers and government agencies, universities, and industry. Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media. Customized laboratory procedures and analyses commonly are used to characterize non-routine samples including, but not limited to, organic and inorganic components in petroleum source rocks, ore and mine waste, clay minerals, and glassy phases. Procedures can be adapted to meet a variety of research objectives.

Spheroidization of molybdenum powder by radio frequency thermal plasma

NASA Astrophysics Data System (ADS)

Liu, Xiao-ping; Wang, Kuai-she; Hu, Ping; Chen, Qiang; Volinsky, Alex A.

2015-11-01

To control the morphology and particle size of dense spherical molybdenum powder prepared by radio frequency (RF) plasma from irregular molybdenum powder as a precursor, plasma process parameters were optimized in this paper. The effects of the carrier gas flow rate and molybdenum powder feeding rate on the shape and size of the final products were studied. The molybdenum powder morphology was examined using high-resolution scanning electron microscopy. The powder phases were analyzed by X-ray diffraction. The tap density and apparent density of the molybdenum powder were investigated using a Hall flow meter and a Scott volumeter. The optimal process parameters for the spherical molybdenum powder preparation are 50 g/min powder feeding rate and 0.6 m3/h carrier gas rate. In addition, pure spherical molybdenum powder can be obtained from irregular powder, and the tap density is enhanced after plasma processing. The average size is reduced from 72 to 62 µm, and the tap density is increased from 2.7 to 6.2 g/cm3. Therefore, RF plasma is a promising method for the preparation of high-density and high-purity spherical powders.

Compositional Tuning, Crystal Growth, and Magnetic Properties of Iron Phosphate Oxide

NASA Astrophysics Data System (ADS)

Tarne, Michael

Iron phosphate oxide, Fe3PO4O 3, is a crystalline solid featuring magnetic Fe3+ ions on a complex lattice composed of closely-spaced triangles. Previous work from our research group on this compound has proposed a helical magnetic structure below T = 163 K attributed to J1 - J2 competing interactions between nearest-neighbor and next-nearest-neighbor iron atoms. This was based on neutron powder diffraction featuring unique broad, flat-topped magnetic reflections due to needle-like magnetic domains. In order to confirm the magnetic structure and origins of frustration, this thesis will expand upon the research focused on this compound. The first chapter focuses on single crystal growth of Fe3PO 4O3. While neutron powder diffraction provides insight to the magnetic structure, powder and domain averaging obfuscate a conclusive structure for Fe3PO4O3 and single crystal neutron scattering is necessary. Due to the incongruency of melting, single crystal growth has proven challenging. A number of techniques including flux growth, slow cooling, and optical floating zone growth were attempted and success has been achieved via heterogenous chemical vapor transport from FePO 4 using ZrCl4 as a transport agent. These crystals are of sufficient size for single crystal measurements on modern neutron diffractometers. Dilution of the magnetic sublattice in frustrated magnets can also provide insight into the nature of competing spin interactions. Dilution of the Fe 3+ lattice in Fe3PO4O3 is accomplished by substituting non-magnetic Ga3+ to form the solid solution series Fe3-xGaxPO4O3 with x = 0, 0.012, 0.06, 0.25, 0.5, 1.0, 1.5. The magnetic susceptibility and neutron powder diffraction data of these compounds are presented. A dramatic decrease of the both the helical pitch length and the domain size is observed with increasing x; for x > 0.5, the compounds lack long range magnetic order. The phases that do exhibit magnetic order show a decrease in helical pitch with increasing x as determined from the magnitude of the magnetic propagation vector. This trend can be qualitatively reproduced by increasing the ratio of J2/ J1 in the Heisenberg model. Intriguingly, the domain size extracted from peak broadening of the magnetic reflections is nearly equal to the pitch length for each value of x, which suggests that the two qualities are linked in this unusual antiferromagnet. The last chapter focuses on the oxyfluoride Fe3PO7-x Fx. Through fluorination using low-temperature chimie douce reactions with polytetrafluoroethylene, the magnetic properties show changes in the magnetic susceptibility, isothermal magnetization, and neutron powder diffraction. The magnetic susceptibility shows a peak near T = 13 K and a zero field cooled/field cooled splitting at T = 78 K. The broad, flat-topped magnetic reflections in the powder neutron diffraction exhibit a decrease in width and increase in intensity. The changes in the neutron powder diffraction suggest an increase in correlation length in the ab plane of the fluorinated compound. Iron phosphate oxide is a unique lattice showing a rich magnetic phase diagram in both the gallium-substituted and fluorinated species. While mean-field interactions are sufficient to describe interactions in the solid solution series Fe3-xGaxPO4O3, the additional magnetic transitions in Fe3PO7-xFx suggest a more complicated set of interactions.

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

PubMed

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

2016-01-01

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

Micron Scale Mineralogy

NASA Astrophysics Data System (ADS)

Caldwell, W. A.; Tamura, N.; Celestre, R. S.; Padmore, H. A.; Patel, J. R.

2002-12-01

Although x-ray diffraction has been used for nearly a century as the mineralogist's definitive tool in determining crystalline structures, it has proved impossible to use this technique to spatially resolve the highly heterogeneous nature of many minerals at the mesoscopic level. Due to recent revolutions in the brightness of x-ray sources and in our ability to focus x-rays, we can now carry out conventional monochromatic rotation crystallography as well as Laue diffraction with sub-micron spatial resolution and produce maps of orientation, strain, mineral type, and even chemical speciation over tens of microns in a short amount of time. We have pioneered the development of these techniques at the 3rd generation synchrotron radiation source (Advanced Light Source) in Berkeley, and will describe their application to understanding the structure of a quartz-geode. Our results show the manner in which grain structure and texture change as a function of distance from the cavity wall and are compared with models of crystal growth in such systems. This example highlights the great utility of a synchrotron based x-ray micro-diffraction beamline and the possibilities it opens to the mineralogist.

Expression, purification, crystallization and preliminary X-ray analysis of conjugated polyketone reductase C2 (CPR-C2) from Candida parapsilosis IFO 0708

PubMed Central

Yamamura, Akihiro; Maruoka, Shintaro; Ohtsuka, Jun; Miyakawa, Takuya; Nagata, Koji; Kataoka, Michihiko; Kitamura, Nahoko; Shimizu, Sakayu; Tanokura, Masaru

2009-01-01

Conjugated polyketone reductase C2 (CPR-C2) from Candida parapsilosis IFO 0708 is a member of the NADPH-dependent aldo-keto reductase (AKR) superfamily and catalyzes the stereospecific reduction of ketopantoyl lactone to d-pantoyl lactone. A diffraction-quality crystal of recombinant CPR-C2 was obtained by the sitting-drop vapour-diffusion method using PEG 3350 as the precipitant. The crystal diffracted X-rays to 1.7 Å resolution on beamline NW12A of the Photon Factory-Advanced Ring (Tsukuba, Japan). The crystal belonged to space group P212121, with unit-cell parameters a = 55.02, b = 68.30, c = 68.93 Å. The Matthews coefficient (V M = 1.76 Å3 Da−1) indicated that the crystal contained one CPR-C2 molecule per asymmetric unit. PMID:19923737

Expression, purification, crystallization and preliminary X-ray analysis of conjugated polyketone reductase C2 (CPR-C2) from Candida parapsilosis IFO 0708.

PubMed

Yamamura, Akihiro; Maruoka, Shintaro; Ohtsuka, Jun; Miyakawa, Takuya; Nagata, Koji; Kataoka, Michihiko; Kitamura, Nahoko; Shimizu, Sakayu; Tanokura, Masaru

2009-11-01

Conjugated polyketone reductase C2 (CPR-C2) from Candida parapsilosis IFO 0708 is a member of the NADPH-dependent aldo-keto reductase (AKR) superfamily and catalyzes the stereospecific reduction of ketopantoyl lactone to d-pantoyl lactone. A diffraction-quality crystal of recombinant CPR-C2 was obtained by the sitting-drop vapour-diffusion method using PEG 3350 as the precipitant. The crystal diffracted X-rays to 1.7 angstrom resolution on beamline NW12A of the Photon Factory-Advanced Ring (Tsukuba, Japan). The crystal belonged to space group P2(1)2(1)2(1), with unit-cell parameters a = 55.02, b = 68.30, c = 68.93 angstrom. The Matthews coefficient (V(M) = 1.76 angstrom(3) Da(-1)) indicated that the crystal contained one CPR-C2 molecule per asymmetric unit.

Non-invasive characterisation of SIX Japanese hand-guards (tsuba)

NASA Astrophysics Data System (ADS)

Barzagli, Elisa; Grazzi, Francesco; Civita, Francesco; Scherillo, Antonella; Pietropaolo, Antonino; Festa, Giulia; Zoppi, Marco

2013-12-01

In this work we present a systematic study of Japanese sword hand-guards ( tsuba) carried out by means of non-invasive techniques using neutrons. Several tsuba from different periods, belonging to the Japanese Section of the Stibbert Museum, were analysed using an innovative approach to characterise the bulk of the samples, coupling two neutron techniques, namely Time of Flight Neutron Diffraction (ToF-ND) and Nuclear Resonance Capture Analysis (NRCA). The measurements were carried out on the same instrument: the INES beam-line at the ISIS spallation pulsed neutron source (UK). NRCA analysis allows identifying the elements present in the sample gauge volume, while neutron diffraction is exploited to quantify the phase distribution and other micro-structural parameters of the metal specimen. The results show that all samples are made of high-quality metal, either steel or copper alloy, with noticeable changes in composition and working techniques, depending on the place and time of manufacturing.

New Insights on the Recrystallization and New Growth of Extensively Radiation-damaged Zircon

NASA Astrophysics Data System (ADS)

Hanchar, J. M.; Schmitz, M. D.; Wirth, R.

2012-12-01

Approximately 10 grams of cm-sized nearly metamict zircon crystals from the Saranac Prospect in the Bancroft District of Ontario were combined by breaking into small pieces and then ground under ethanol to a fine powder with an agate mortar and pestle in order to make enough homogeneously mixed material for multiple powder X-Ray and diffraction scans, high-resolution transmission electron microscopy (HR-TEM) measurements, and chemical abrasion isotope dilution thermal ionization mass spectrometry (CA-TIMS). While these large zircon crystals ground to a powder have a larger surface area and not in the same physical state (i.e., brown and metamict) as what is typically analyzed in single zircon CA-ID-TIMS U-Pb analysis (clear euhedral grains), the physical and chemical changes that occur during the heat treatment used in CA-TIMS are thought to be similar processes. Aliquots of the ground zircon powder were annealed in situ using a Pt furnace in a powder diffractometer during which time simultaneous powder diffraction patterns were acquired starting at 25°C, at elevated temperature (from 500°C to 1400°C) at selected time intervals, and then again at 25°C. The powder X-ray diffraction results indicate that below ~900°C the recrystallization of the zircon powder commences but is incomplete, even after 36 hours, with diffuse low intensity diffraction peaks. At 1150°C the zircon powder shows significant recrystallization. At 1150°C, the recrystallization is essentially complete in less than one hour. Before heating the zircon powder samples consisted of clear, transparent to brown, translucent, complexly zoned fragments. After heating at 900°C the zircon powder retained a smaller percentage of clear or brown complexly zoned fragments, while the majority of material had transformed to oscillatory or irregularly zoned, dominantly white opaque microcrystalline fragments. The clear fragments were hypothesized to be preexisting original crystalline zircon, the brown complexly zoned fragments preexisting metamict zircon, and the white opaque fragment new recrystallized zircon and other oxides. At 1150°C all that remained after heating were dominantly white opaque fragments and extremely rare clear fragments. A variety of fragment types from unannealed, 900°C and 1150°C anneals were chemically abraded in concentrated hydrofluoric acid at 190°C for 12 hours. Upon treatment with chemical abrasion, all unannealed material, nearly all material from the 900°C anneal, and all white opaque microcrystalline material from the 1150°C anneal dissolved; only the rare residual clear, transparent fragments from the 1150°C anneal were robust to chemical abrasion at these conditions. Residual clear fragments yielded concordant U-Pb ID-TIMS dates of 1064 Ma (considering updated U decay constant ratio), confirming the hypothesis that low-U closed system domains are preserved through annealing up to 1150°C and can be extracted via chemical abrasion from even dominantly metamict zircon crystals. By contrast, newly formed crystallites resulting from metamict zircon breakdown during annealing appear to be quite soluble during chemical abrasion. Further experiments are underway to refine minimum threshold chemical abrasion conditions necessary to eliminate open-system domains in the Saranac zircon.

Phase modification of copper phthalocyanine semiconductor by converting powder to thin film

NASA Astrophysics Data System (ADS)

Ai, Xiaowei; Lin, Jiaxin; Chang, Yufang; Zhou, Lianqun; Zhang, Xianmin; Qin, Gaowu

2018-01-01

Thin films of copper phthalocyanine (CuPc) semiconductor were deposited on glass substrates by a thermal evaporation system using the CuPc powder in a high vacuum. The crystal structures of both the films and the powder were measured by the X-ray diffraction spectroscopy technique. It is observed that CuPc films only show one peak at 6.84°, indicating a high texture of α phase along (200) orientation. In comparison, CuPc powder shows a series of peaks, which are confirmed from the mixture of both α and β phases. The effects of substrate anneal temperature on the film structure, grain size and optical absorption property of CuPc films were also investigated. All the films are of α phase and the full width of half maximum for (200) diffraction peak becomes narrow with increasing the substrate temperatures. The average grain size calculated by the Scherrer's formula is 33.63 nm for the film without anneal, which is increased up to 58.29 nm for the film annealed at 200 °C. Scanning electron microscope was further measured to prove the growth of crystalline grain and to characterize the morphologies of CuPc films. Ultraviolet-visible absorption spectra were employed to study the structure effect on the optical properties of both CuPc films and powder. Fourier Transform infrared spectroscopy was used to identify the crystalline nature of both CuPc powder and film.

Fabrication of Spherical AlSi10Mg Powders by Radio Frequency Plasma Spheroidization

NASA Astrophysics Data System (ADS)

Wang, Linzhi; Liu, Ying; Chang, Sen

2016-05-01

Spherical AlSi10Mg powders were prepared by radio frequency plasma spheroidization from commercial AlSi10Mg powders. The fabrication process parameters and powder characteristics were investigated. Field emission scanning electron microscope, X-ray diffraction, laser particle size analyzer, powder rheometer, and UV/visible/infrared spectrophotometer were used for analyses and measurements of micrographs, phases, granulometric parameters, flowability, and laser absorption properties of the powders, respectively. The results show that the obtained spherical powders exhibit good sphericity, smooth surfaces, favorable dispersity, and excellent fluidity under appropriate feeding rate and flow rate of carrier gas. Further, acicular microstructures of the spherical AlSi10Mg powders are composed of α-Al, Si, and a small amount of Mg2Si phase. In addition, laser absorption values of the spherical AlSi10Mg powders increase obviously compared with raw material, and different spectra have obvious absorption peaks at a wavelength of about 826 nm.

Defect ordering in YBa 2Cu 3O 6.5 and YBa 2Cu 3O 6.6: Synthesis and characterization by neutron and electron diffraction

NASA Astrophysics Data System (ADS)

Lin, Y. P.; Greedan, J. E.; O'Reilly, A. H.; Reimers, J. N.; Stager, C. V.; Post, M. L.

1990-02-01

Polycrystalline samples of YBa 2Cu 3O 6.5 and YBa 2Cu 3O 6.6 were prepared by oxygen titration of YBa 2 Cu 3O 6.0 at 450°C followed by slow cooling to room temperature. Both samples showed evidence for the a' = 2a supercell in individual grains by electron diffraction as reported previously. In addition the superlattice was observed in neutron powder diffraction indicating that the bulk material is also well ordered. In this study the YBa 2Cu 3O 6.6 phase showed longer correlation lengths for ordering along both a* and b* than YBa 2Cu 3O 6.5. For the former compound the powder-averaged, sample-averaged a* correlation distance is 26A˚from neutron diffraction. Analysis of electron diffraction profiles on selected single crystals give correlation lengths along a*, b*, and c* of 100, 200, and 50A˚, respectively. Dark field imaging discloses the presence of striped, ordered domains elongated along b* with a distribution of sizes. Both neutron diffraction and dark field imaging indicate that the volume fraction of the ordered domains is about 50%. A correlation is noted between the Meissner Effect and the extent of defect ordering in the bulk samples of the two phases.

The storage degradation of an 18650 commercial cell studied using neutron powder diffraction

NASA Astrophysics Data System (ADS)

Lee, Po-Han; Wu, She-huang; Pang, Wei Kong; Peterson, Vanessa K.

2018-01-01

Commercial 18650 lithium ion cells containing a blended positive electrode of layered LiNi0.5Mn0.3Co0.2O2 and spinel Li1.1Mn1.9O4 alongside a graphite negative electrode were stored at various depth-of-discharge (DoD) at 60 °C for 1, 2, 4, and 6 months. After storage, the cells were cycled at C/25 at 25 °C between 2.75 and 4.2 V for capacity determination and incremental capacity analysis (ICA). In addition to ICA analysis, the mechanism for capacity fade was investigated by combining the results of neutron powder diffraction under in-situ and operando conditions, in conjunction with post-mortem studies of the electrodes using synchrotron X-ray powder diffraction and inductively-coupled plasma optical emission spectroscopy. Among the cells, those stored at 25% DoD suffered the highest capacity fade due to their higher losses of active Li, NMC, and LMO than cells stored at other DoD. The cells stored at 0% DoD shows second high capacity fade because they exhibit the highest of active LMO and graphite anode among the stored cells and higher losses of active Li and NMC than cells stored at 50% DoD.

Fatigue of LiNi0.8Co0.15Al0.05O2 in commercial Li ion batteries

NASA Astrophysics Data System (ADS)

Kleiner, Karin; Dixon, Ditty; Jakes, Peter; Melke, Julia; Yavuz, Murat; Roth, Christina; Nikolowski, Kristian; Liebau, Verena; Ehrenberg, Helmut

2015-01-01

The degradation of LiNi0.8Co0.15Al0.05O2 (LNCAO), a cathode material in lithium-ion-batteries, was studied using in situ powder diffraction and in situ Ni K edge X-ray absorption spectroscopy (XAS). The fatigued material was taken from a 7 Ah battery which was cycled for 34 weeks under defined durability conditions. Meanwhile, a cell was stored, as reference, under controlled conditions without electrochemical treatment. The fatigued LNCAO used in this study showed a capacity loss of 26% ± 9% compared to the non-cycled material. During charge and discharge the local and the overall structure of LNCAO was investigated by X-ray near edge structure (XANES) analysis, the extended X-ray absorption fine structure (EXAFS) analysis and by using Rietveld refinement of in situ powder diffraction patterns. Both powder diffraction and XAS revealed additional, rhombohedral phases which do not change with electrochemical cycling. Moreover, a phase with the lattice parameters of fully lithiated LNCAO was still present in the fatigued material at high potentials, while it was absent in the non-fatigued reference material. The coexistence of these phases is described by domains within the LNCAO particles, in correlation with the observed fatigue.

Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

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

Post,J.; Bish, D.; Heaney, P.

2007-01-01

Rietveld refinements using synchrotron powder X-ray diffraction data were used to study the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room-temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic H{sub 2}O site. The RT structure under vacuum retained only {approx}1/8 of the zeolitic H{sub 2}O and the volume decreased by 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic H{sub 2}O is lost bymore » {approx}390 K, accompanied by a decrease in the a and c unit-cell parameters. Above {approx}600 K the sepiolite structure folds as one-half of the crystallographically bound H{sub 2}O is lost. Rietveld refinements of the 'anhydrous' sepiolite structure reveal that, in general, unit-cell parameters a and b and volume steadily decrease with increasing temperature; there is an obvious change in slope at {approx}820 K suggesting a phase transformation coinciding with the loss of the remaining bound H{sub 2}O molecule.« less

Phase Equilibria and Crystallography of Ceramic Oxides

PubMed Central

Wong-Ng, W.; Roth, R. S.; Vanderah, T. A.; McMurdie, H. F.

2001-01-01

Research in phase equilibria and crystallography has been a tradition in the Ceramics Division at National Bureau of Standards/National Institute of Standatrds and Technology (NBS/NIST) since the early thirties. In the early years, effort was concentrated in areas of Portland cement, ceramic glazes and glasses, instrument bearings, and battery materials. In the past 40 years, a large portion of the work was related to electronic materials, including ferroelectrics, piezoelectrics, ionic conductors, dielectrics, microwave dielectrics, and high-temperature superconductors. As a result of the phase equilibria studies, many new compounds have been discovered. Some of these discoveries have had a significant impact on US industry. Structure determinations of these new phases have often been carried out as a joint effort among NBS/NIST colleagues and also with outside collaborators using both single crystal and neutron and x-ray powder diffraction techniques. All phase equilibria diagrams were included in Phase Diagrams for Ceramists, which are collaborative publications between The American Ceramic Society (ACerS) and NBS/NIST. All x-ray powder diffraction patterns have been included in the Powder Diffraction File (PDF). This article gives a brief account of the history of the development of the phase equilibria and crystallographic research on ceramic oxides in the Ceramics Division. Represented systems, particularly electronic materials, are highlighted. PMID:27500068

Effects of limestone petrography and calcite microstructure on OPC clinker raw meals burnability

NASA Astrophysics Data System (ADS)

Galimberti, Matteo; Marinoni, Nicoletta; Della Porta, Giovanna; Marchi, Maurizio; Dapiaggi, Monica

2017-10-01

Limestone represents the main raw material for ordinary Portland cement clinker production. In this study eight natural limestones from different geological environments were chosen to prepare raw meals for clinker manufacturing, aiming to define a parameter controlling the burnability. First, limestones were characterized by X-Ray Fluorescence, X-Ray Powder Diffraction and Optical Microscopy to assess their suitability for clinker production and their petrographic features. The average domains size and the microstrain of calcite were also determined by X-Ray Powder Diffraction line profile analysis. Then, each limestone was admixed with clay minerals to achieve the adequate chemical composition for clinker production. Raw meals were thermally threated at seven different temperatures, from 1000 to 1450 °C, to evaluate their behaviour on heating by ex situ X-Ray Powder Diffraction and to observe the final clinker morphology by Scanning Electron Microscopy. Results indicate the calcite microstrain is a reliable parameter to predict the burnability of the raw meals, in terms of calcium silicates growth and lime consumption. In particular, mixtures prepared starting from high-strained calcite exhibit a better burnability. Later, when the melt appears this correlation vanishes; however differences in the early burnability still reflect on the final clinker composition and texture.

Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying

NASA Astrophysics Data System (ADS)

Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

2015-12-01

Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The tetracalcium phosphate phase was homogeneous; the apatite phase contained defects localized on the sixfold axis and consisted of hydroxyapatite and oxyapatite. Technological factors contributing to the transformation of hydroxyapatite powder structure during coating formation by detonation spraying are discussed.

Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying.

PubMed

Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

2015-12-01

Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The tetracalcium phosphate phase was homogeneous; the apatite phase contained defects localized on the sixfold axis and consisted of hydroxyapatite and oxyapatite. Technological factors contributing to the transformation of hydroxyapatite powder structure during coating formation by detonation spraying are discussed.

Synthesis of Cu-W nanocomposite by high-energy ball milling.

PubMed

Venugopal, T; Rao, K Prasad; Murty, B S

2007-07-01

The Cu-W bulk nanocomposites of different compositions were successfully synthesized by high-energy ball milling of elemental powders. The nanocrystalline nature of the Cu-W composite powder is confirmed by X-ray diffraction analysis, transmission electron microscopy, and atomic force microscopy. The Cu-W nanocomposite powder could be sintered at 300-400 degrees C below the sintering temperature of the un-milled Cu-W powders. The Cu-W nanocomposites showed superior densification and hardness than that of un-milled Cu-W composites. The nanocomposites also have three times higher hardness to resistivity ratio in comparison to Oxygen free high conductivity copper.

Advances in indirect detector systems for ultra high-speed hard X-ray imaging with synchrotron light

NASA Astrophysics Data System (ADS)

Olbinado, M. P.; Grenzer, J.; Pradel, P.; De Resseguier, T.; Vagovic, P.; Zdora, M.-C.; Guzenko, V. A.; David, C.; Rack, A.

2018-04-01

We report on indirect X-ray detector systems for various full-field, ultra high-speed X-ray imaging methodologies, such as X-ray phase-contrast radiography, diffraction topography, grating interferometry and speckle-based imaging performed at the hard X-ray imaging beamline ID19 of the European Synchrotron—ESRF. Our work highlights the versatility of indirect X-ray detectors to multiple goals such as single synchrotron pulse isolation, multiple-frame recording up to millions frames per second, high efficiency, and high spatial resolution. Besides the technical advancements, potential applications are briefly introduced and discussed.

The ID23-2 structural biology microfocus beamline at the ESRF

PubMed Central

Flot, David; Mairs, Trevor; Giraud, Thierry; Guijarro, Matias; Lesourd, Marc; Rey, Vicente; van Brussel, Denis; Morawe, Christian; Borel, Christine; Hignette, Olivier; Chavanne, Joel; Nurizzo, Didier; McSweeney, Sean; Mitchell, Edward

2010-01-01

The first phase of the ESRF beamline ID23 to be constructed was ID23-1, a tunable MAD-capable beamline which opened to users in early 2004. The second phase of the beamline to be constructed is ID23-2, a monochromatic microfocus beamline dedicated to macromolecular crystallography experiments. Beamline ID23-2 makes use of well characterized optical elements: a single-bounce silicon (111) monochromator and two mirrors in Kirkpatrick–Baez geometry to focus the X-ray beam. A major design goal of the ID23-2 beamline is to provide a reliable, easy-to-use and routine microfocus beam. ID23-2 started operation in November 2005, as the first beamline dedicated to microfocus macromolecular crystallography. The beamline has taken the standard automated ESRF macromolecular crystallography environment (both hardware and software), allowing users of ID23-2 to be rapidly familiar with the microfocus environment. This paper describes the beamline design, the special considerations taken into account given the microfocus beam, and summarizes the results of the first years of the beamline operation. PMID:20029119

Neutron diffraction studies for realtime leaching of catalytic Ni

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

Iles, Gail N., E-mail: gail.iles@helmholtz-berlin.de; Reinhart, Guillaume, E-mail: guillaume.reinhart@im2np.fr; Institut Laue-Langevin, 6 rue Jules Horowitz, BP 156, 38042 Grenoble

2014-07-21

The leaching of Al from intermetallic samples of Nickel Aluminium alloys to form Raney-type nickel catalysts is widely used in the hydrogenation industry, however, little is known of the leaching process itself. In this study, the leaching of Al was measured in realtime, in situ, using the high-flux powder neutron diffractometer, D20, at the Institut Laue-Langevin. Despite the liberation of hydrogen and effervescent nature of the reaction the transformation of the dry powder phases into Raney-type Ni was determined. Samples produced by gas-atomisation were found to leach faster than those produced using the cast and crushed technique. Regardless of processingmore » route of the precursor powder, the formation of spongy-Ni occurs almost immediately, while Ni{sub 2}Al{sub 3} and NiAl{sub 3} continue to transform over longer periods of time. Small-angle scattering and broadening of the diffraction peaks is an evidence for the formation of the smaller Ni particles. Understanding the kinetics of the leaching process will allow industry to refine production of catalysts for optimum manufacturing time while knowledge of leaching dynamics of powders produced by different manufacturing techniques will allow further tailoring of catalytic materials.« less

The synthesis of nanostructured SiC from waste plastics and silicon powder

NASA Astrophysics Data System (ADS)

Ju, Zhicheng; Xu, Liqiang; Pang, Qiaolian; Xing, Zheng; Ma, Xiaojian; Qian, Yitai

2009-09-01

Waste plastics constitute a growing environmental problem. Therefore, the treatment of waste plastics should be considered. Here we synthesize 3C-SiC nanomaterials coexisting with amorphous graphite particles utilizing waste plastics and Si powder at 350-500 °C in a stainless steel autoclave. 3C-SiC could be finally obtained after refluxing with aqueous HClO4 (70 wt%) at 180 °C. X-ray powder diffraction patterns indicate that the product is 3C-SiC with the calculated lattice constant a = 4.36 Å. Transmission electron microscopy (TEM) images show that the SiC samples presented two morphologies: hexagonal platelets prepared by the waste detergent bottles or beverage bottles and nanowires prepared by waste plastic bags respectively. The corresponding selected area electron diffraction (SAED) pattern indicates that either the entire hexagonal platelet or the nanowire is single crystalline. High-resolution TEM shows the planar surfaces of the SiC platelet correspond to {111} planes; the lateral surfaces are {110} planes and the preferential growth direction of the nanowires is along [111]. The output of SiC was ~39% based on the amount of Si powder.

Upconversion luminescence of Er3+/Yb3+ doped Sr5(PO4)3OH phosphor powders

NASA Astrophysics Data System (ADS)

Mokoena, P. P.; Swart, H. C.; Ntwaeaborwa, O. M.

2018-04-01

Sr5(PO4)3OH co-doped with Er3+and Yb3+ powder phosphors were synthesized by urea combustion method. The crystal structure was analyzed using X-ray diffraction (XRD). Particle morphology was analyzed using a Jeol JSM 7800F thermal field emission scanning electron microscope (FE-SEM) and the chemical composition analysis was carried out using an Oxford Instruments AzTEC energy dispersive spectrometer (EDS) attached to the FE-SEM. Upconversion emission was measured by using a FLS980 Spectrometer equipped with a 980 nm NIR laser as the excitation source, and a photomultiplier (PMT) detector. The XRD data of the Sr5(PO4)3OH powder exhibited characteristic diffraction patterns of the hexagonal structure referenced in the standard JCPDS card number 00-033-1348. The sharp peaks revealed the formation of crystalline Sr5(PO4)3OH. The powders were made up of hexagonal nanospheres. The enhanced red emission due to the 4F9/2 → 4I15/2 transitions of Er3+ was observed and was attributed to up conversion (UC) energy transfer from Yb3+. The upconversion energy transfer mechanism from Yb3+ to Er3+ is discussed.

Green biosynthesis of silver nanoparticles using Curcuma longa tuber powder

PubMed Central

Shameli, Kamyar; Ahmad, Mansor Bin; Zamanian, Ali; Sangpour, Parvanh; Shabanzadeh, Parvaneh; Abdollahi, Yadollah; Zargar, Mohsen

2012-01-01

Green synthesis of noble metal nanoparticles is a vastly developing area of research. Metallic nanoparticles have received great attention from chemists, physicists, biologists, and engineers who wish to use them for the development of a new-generation of nanodevices. In this study, silver nanoparticles were biosynthesized from aqueous silver nitrate through a simple and eco-friendly route using Curcuma longa tuber-powder extracts, which acted as a reductant and stabilizer simultaneously. Characterizations of nanoparticles were done using different methods, which included ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray fluorescence spectrometry, and Fourier-transform infrared spectroscopy. The ultraviolet-visible spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 415 nm. Transmission electron microscopy showed that mean diameter and standard deviation for the formation of silver nanoparticles was 6.30 ± 2.64 nm. Powder X-ray diffraction showed that the particles are crystalline in nature, with a face-centered cubic structure. The most needed outcome of this work will be the development of value-added products from C. longa for biomedical and nanotechnology-based industries. PMID:23341739

Secondary Mineral Formation Associated With Respiration of Nontronite, NAu-1 by Iron Reducing Bacteria

DTIC Science & Technology

2005-12-01

with a set of expected powder diffraction rings for siderite (JCPDS Card 8-133). The diffraction rings correspond to the d-spacing values (and hkl ...Bender et al., Geochim. Cos- 33j. E. Kostka and K. H. Nealson, in Techniques in Microbial Ecology, mochim. Acta 43(7), 1075 (1979). edited by R. S

Neutron diffraction measurements and micromechanical modelling of temperature-dependent variations in TATB lattice parameters

DOE PAGES

Yeager, John D.; Luscher, Darby J.; Vogel, Sven C.; ...

2016-02-02

Triaminotrinitrobenzene (TATB) is a highly anisotropic molecular crystal used in several plastic-bonded explosive (PBX) formulations. TATB-based explosives exhibit irreversible volume expansion (“ratchet growth”) when thermally cycled. A theoretical understanding of the relationship between anisotropy of the crystal, crystal orientation distribution (texture) of polycrystalline aggregates, and the intergranular interactions leading to this irreversible growth is necessary to accurately develop physics-based predictive models for TATB-based PBXs under various thermal environments. In this work, TATB lattice parameters were measured using neutron diffraction during thermal cycling of loose powder and a pressed pellet. The measured lattice parameters help clarify conflicting reports in the literaturemore » as these new results are more consistent with one set of previous results than another. The lattice parameters of pressed TATB were also measured as a function of temperature, showing some differences from the powder. This data is used along with anisotropic single-crystal stiffness moduli reported in the literature to model the nominal stresses associated with intergranular constraints during thermal expansion. The texture of both specimens were characterized and the pressed pellet exhibits preferential orientation of (001) poles along the pressing direction, whereas no preferred orientation was found for the loose powder. Lastly, thermal strains for single-crystal TATB computed from lattice parameter data for the powder is input to a self-consistent micromechanical model, which predicts the lattice parameters of the constrained TATB crystals within the pellet. The agreement of these model results with the diffraction data obtained from the pellet is discussed along with future directions of research.« less

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

NASA Astrophysics Data System (ADS)

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; Martin, Aiden A.; Depond, Philip J.; Guss, Gabriel M.; Thampy, Vivek; Fong, Anthony Y.; Weker, Johanna Nelson; Stone, Kevin H.; Tassone, Christopher J.; Kramer, Matthew J.; Toney, Michael F.; Van Buuren, Anthony; Matthews, Manyalibo J.

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ˜1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ˜50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes.

PubMed

Calta, Nicholas P; Wang, Jenny; Kiss, Andrew M; Martin, Aiden A; Depond, Philip J; Guss, Gabriel M; Thampy, Vivek; Fong, Anthony Y; Weker, Johanna Nelson; Stone, Kevin H; Tassone, Christopher J; Kramer, Matthew J; Toney, Michael F; Van Buuren, Anthony; Matthews, Manyalibo J

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ∼1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ∼50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

Empirically testing vaterite structural models using neutron diffraction and thermal analysis

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

Chakoumakos, Bryan C.; Pracheil, Brenda M.; Koenigs, Ryan

Otoliths, calcium carbonate (CaCO 3) ear bones, are among the most commonly used age and growth structures of fishes. Most fish otoliths are comprised of the most dense CaCO 3 polymorph, aragonite. Sturgeon otoliths, in contrast, have been characterized as the rare and structurally enigmatic polymorph, vaterite a metastable polymorph of CaCO 3. Vaterite is an important material ranging from biomedical to personal care applications although its crystal structure is highly debated. We characterized the structure of sturgeon otoliths using thermal analysis and neutron powder diffraction, which is used non-destructively. We confirmed that while sturgeon otoliths are primarily composed ofmore » vaterite, they also contain the denser CaCO 3 polymorph, calcite. For the vaterite fraction, neutron diffraction data provide enhanced discrimination of the carbonate group compared to x-ray diffraction data, owing to the different relative neutron scattering lengths, and thus offer the opportunity to uniquely test the more than one dozen crystal structural models that have been proposed for vaterite. Of those, space group P6 522 model, a = 7.1443(4)Å , c = 25.350(4)Å , V = 1121.5(2)Å 3 provides the best fit to the neutron powder diffraction data, and allows for a structure refinement using rigid carbonate groups.« less

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

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

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« less

Empirically testing vaterite structural models using neutron diffraction and thermal analysis

DOE PAGES

Chakoumakos, Bryan C.; Pracheil, Brenda M.; Koenigs, Ryan; ...

2016-11-18

Otoliths, calcium carbonate (CaCO 3) ear bones, are among the most commonly used age and growth structures of fishes. Most fish otoliths are comprised of the most dense CaCO 3 polymorph, aragonite. Sturgeon otoliths, in contrast, have been characterized as the rare and structurally enigmatic polymorph, vaterite a metastable polymorph of CaCO 3. Vaterite is an important material ranging from biomedical to personal care applications although its crystal structure is highly debated. We characterized the structure of sturgeon otoliths using thermal analysis and neutron powder diffraction, which is used non-destructively. We confirmed that while sturgeon otoliths are primarily composed ofmore » vaterite, they also contain the denser CaCO 3 polymorph, calcite. For the vaterite fraction, neutron diffraction data provide enhanced discrimination of the carbonate group compared to x-ray diffraction data, owing to the different relative neutron scattering lengths, and thus offer the opportunity to uniquely test the more than one dozen crystal structural models that have been proposed for vaterite. Of those, space group P6 522 model, a = 7.1443(4)Å , c = 25.350(4)Å , V = 1121.5(2)Å 3 provides the best fit to the neutron powder diffraction data, and allows for a structure refinement using rigid carbonate groups.« less

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

DOE PAGES

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; ...

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« less

Template-free solution approach to synthesize CdS dendrites with SCN based ionic liquid

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

Li, Kangfeng; Li, Jiajia; Cheng, Xianyi

2011-07-15

Highlights: {yields} Template-free solution approach to synthesize CdS hierarchical dendrites. {yields} The 1-butyl-3-methlyimidazole thiocyanate ([BMIM][SCN]) plays doubly functional roles in the progress. {yields} The CdS hierarchical dendrites exhibit a more intense emission at 710 nm belongs to infrared band. -- Abstract: Cadmium sulfide dendrites were synthesized by a facile hydrothermal treatment from CdCl{sub 2} and ionic liquid 1-butyl-3-methlyimidazole thiocyanate acted both as sulfur source and surfactant. The product was characterized by means of X-ray powder diffraction and scanning electron microscopy. X-ray powder diffraction studies indicated that the product was well-crystallized hexagonal phase of CdS, and the scanning electron microscopy imagesmore » showed that the obtained powders consisted of a wealth of well-defined CdS dendritic microstructures with a pronounced trunk and highly ordered branches. The UV-Vis and photoluminescence spectroscopy measurements were taken as well. The possible formation mechanism of CdS dendrites was simply proposed in the end.« less

Driving forces of redistribution of elements during quasicrystalline phase formation under heating of mechanically alloyed Al65Cu23Fe12 powder

NASA Astrophysics Data System (ADS)

Tcherdyntsev, V. V.; Kaloshkin, S. D.; Shelekhov, E. V.; Principi, G.; Rodin, A. O.

2008-02-01

Al65Cu23Fe12 alloys were prepared by ball milling of the elemental powders mixture. Phase and structural transformations at heating of as-milled powders were investigated by X-ray diffraction analysis. Precision analysis of Mössbauer spectra was performed to check the adequacy of the fitting of X-ray diffraction patterns. The results were compared with the data of differential scanning and solution calorimetry, as well as with the thermodynamic literature data, in order to estimate the driving forces of redistribution of elements that preceded the formation of single-phase quasicrystalline structure. The heat of elements mixing, which is positive for Cu-Fe system and negative for Al-Fe and Al-Cu systems, was supposed to be a decisive factor for phase transformations during heating of the alloy. The correlation between sequence of phase transformations during heating and the thermodynamic data was discussed and the scheme describing phase transformations observed was proposed.

Characterization of food additive-potato starch complexes by FTIR and X-ray diffraction.

PubMed

Dankar, Iman; Haddarah, Amira; Omar, Fawaz E L; Pujolà, Montserrat; Sepulcre, Francesc

2018-09-15

Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) techniques were used to study the effect of four food additives, agar, alginate, lecithin and glycerol, at three different concentrations, 0.5, 1 and 1.5%, on the molecular structure of potato puree prepared from commercial potato powder. Vibrational spectra revealed that the amylose-amylopectin skeleton present in the raw potato starch was missing in the potato powder but could be fully recovered upon water addition when the potato puree was prepared. FTIR peaks corresponding to water were clearly present in the potato powder, indicating the important structural role of water molecules in the recovery of the initial molecular conformation. None of the studied puree samples presented a crystalline structure or strong internal order. A comparison of the FTIR and XRD results revealed that the additives exerted some effects, mainly on the long-range order of the starch structure via interacting with and changing -OH and hydrogen bond interactions. Copyright © 2018 Elsevier Ltd. All rights reserved.

High-resolution inelastic neutron scattering and neutron powder diffraction study of the adsorption of dihydrogen by the Cu(II) metal-organic framework material HKUST-1

NASA Astrophysics Data System (ADS)

Callear, Samantha K.; Ramirez-Cuesta, Anibal J.; David, William I. F.; Millange, Franck; Walton, Richard I.

2013-12-01

We present new high-resolution inelastic neutron scattering (INS) spectra (measured using the TOSCA and MARI instruments at ISIS) and powder neutron diffraction data (measured on the diffractometer WISH at ISIS) from the interaction of the prototypical metal-organic framework HKUST-1 with various dosages of dihydrogen gas. The INS spectra show direct evidence for the sequential occupation of various distinct sites for dihydrogen in the metal-organic framework, whose population is adjusted during increasing loading of the guest. The superior resolution of TOSCA reveals subtle features in the spectra, not previously reported, including evidence for split signals, while complementary spectra recorded on MARI present full information in energy and momentum transfer. The analysis of the powder neutron patterns using the Rietveld method shows a consistent picture, allowing the crystallographic indenisation of binding sites for dihydrogen, thus building a comprehensive picture of the interaction of the guest with the nanoporous host.

Fabricating the spherical and flake silver powder used for the optoelectronic devices

NASA Astrophysics Data System (ADS)

Ju, Wei; Ma, Wangjing; Zhang, Fangzhi; Chen, Yixiang; Xie, Jinpeng

2018-01-01

The spherical and flake silver powder with different particle size for the optoelectronic devices was partly prepared by using chemical reduction and ball milling method, and charactered by scanning electron microscope (SEM), X-ray diffraction (XRD), laser particle size analyzer and thermo-gravimetric(TG) analyzer. The particle size of three series of spherical silver powder fabricated by chemical reduction is about 1.5μm, 1μm and 0.6μm, respectively; after being mechanical milling, the particle size of flake silver powder with high flaky rate is about 10μm, 6μm and 2μm respectively. Thermo gravimetric (TG) and XRD analyses showed that the silver powders have high purity and crystalline, and then the laser particle size and SEM analyses showed that the silver powders has good uniformity.

Moisture sorption by cellulose powders of varying crystallinity.

PubMed

Mihranyan, Albert; Llagostera, Assumpcio Piñas; Karmhag, Richard; Strømme, Maria; Ek, Ragnar

2004-01-28

Moisture in microcrystalline cellulose may cause stability problems for moisture sensitive drugs. The aim of this study was to investigate the influence of crystallinity and surface area on the uptake of moisture in cellulose powders. Powders of varying crystallinity were manufactured, and the uptake of moisture was investigated at different relative humidities. The structure of the cellulose powders was characterized by X-ray diffraction, BET surface area analysis, and scanning electron microscopy. Moisture uptake was directly related to the cellulose crystallinity and pore volume: Cellulose powders with higher crystallinity showed lower moisture uptake at relative humidities below 75%, while at higher humidities the moisture uptake could be associated with filling of the large pore volume of the cellulose powder of highest crystallinity. In conclusion, the structure of cellulose should be thoroughly considered when manufacturing low moisture grades of MCC.

Different magnetic origins of (Mn, Fe)-codoped ZnO powders and thin films

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

Fan, Jiuping; Jiang, Fengxian; Quan, Zhiyong

2012-11-15

Graphical abstract: The effects of the sample forms, fabricated methods, and process conditions on the structural and magnetic properties of (Mn, Fe)-codoped ZnO powders and films were systematically studied. The origins of ferromagnetism in the vacuum-annealed powder and PLD-deposited film are different. The former originates from the impurities of magnetic clusters, whereas the latter comes from the almost homogenous phase. Highlights: ► The magnetic natures of Zn{sub 0.98}Mn{sub 0.01}Fe{sub 0.01}O powders and thin films come from different origins. ► The ferromagnetism of the powder is mainly from the contribution of magnetic clusters. ► Whereas the ferromagnetic behavior of the filmmore » comes from the almost homogenous phase. -- Abstract: The structural and magnetic properties of (Mn, Fe)-codoped ZnO powders as well as thin films were investigated. The X-ray diffraction and magnetic measurements indicated that the higher sintering temperature facilitates more Mn and Fe incorporation into ZnO. Magnetic measurements indicated that the powder sintered in air at 800 °C showed paramagnetic, but it exhibited obvious room temperature ferromagnetism after vacuum annealing at 600 °C. The results revealed that magnetic clusters were the major contributors to the observed ferromagnetism in vacuum-annealed Zn{sub 0.98}Mn{sub 0.01}Fe{sub 0.01}O powder. Interestingly, the room temperature ferromagnetism was also observed in the Zn{sub 0.98}Mn{sub 0.01}Fe{sub 0.01}O film deposited via pulsed laser deposition from the air-sintered paramagnetic target, but the secondary phases in the film were not detected from X-ray diffraction, transmission electron microscopy, and zero-field cooling and field cooling. Apparently, the magnetic natures of powders and films come from different origins.« less

Tailoring oxidation of aluminum nanoparticles reinforced with carbon nanotubes

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

Sharma, Manjula; Sharma, Vimal, E-mail: manjula.physics@gmail.com

2016-05-23

In this report, the oxidation temperature and reaction enthalpy of Aluminum (Al) nanoparticles has been controlled by reinforcing with carbon nanotubes. The physical mixing method with ultrasonication was employed to synthesize CNT/Al nanocomposite powders. The micro-morphology of nanoconmposite powders has been analysed by scanning electron microscopy, energy dispersive spectroscopy, Raman spectroscopy and X-ray diffraction techniques. The oxidation behavior of nanocomposite powders analyzed by thermogravimetry/differential scanning calorimertry showed improvement in the exothermic enthalpy. Largest exothermic enthalpy of-1251J/g was observed for CNT (4 wt%)/Al nanocomposite.

Macromolecular powder diffraction : structure solution via molecular.

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

Doebbler, J.; Von Dreele, R.; X-Ray Science Division

Macromolecular powder diffraction is a burgeoning technique for protein structure solution - ideally suited for cases where no suitable single crystals are available. Over the past seven years, pioneering work by Von Dreele et al. [1,2] and Margiolaki et al. [3,4] has demonstrated the viability of this approach for several protein structures. Among these initial powder studies, molecular replacement solutions of insulin and turkey lysozyme into alternate space groups were accomplished. Pressing the technique further, Margiolaki et al. [5] executed the first molecular replacement of an unknown protein structure: the SH3 domain of ponsin, using data from a multianalyzer diffractometer.more » To demonstrate that cross-species molecular replacement using image plate data is also possible, we present the solution of hen egg white lysozyme using the 60% identical human lysozyme (PDB code: 1LZ1) as the search model. Due to the high incidence of overlaps in powder patterns, especially in more complex structures, we have used extracted intensities from five data sets taken at different salt concentrations in a multi-pattern Pawley refinement. The use of image plates severely increases the overlap problem due to lower detector resolution, but radiation damage effects are minimized with shorter exposure times and the fact that the entire pattern is obtained in a single exposure. This image plate solution establishes the robustness of powder molecular replacement resulting from different data collection techniques.« less

Laboratory manual: mineral X-ray diffraction data retrieval/plot computer program

USGS Publications Warehouse

Hauff, Phoebe L.; VanTrump, George

1976-01-01

The Mineral X-Ray Diffraction Data Retrieval/Plot Computer Program--XRDPLT (VanTrump and Hauff, 1976a) is used to retrieve and plot mineral X-ray diffraction data. The program operates on a file of mineral powder diffraction data (VanTrump and Hauff, 1976b) which contains two-theta or 'd' values, and intensities, chemical formula, mineral name, identification number, and mineral group code. XRDPLT is a machine-independent Fortran program which operates in time-sharing mode on a DEC System i0 computer and the Gerber plotter (Evenden, 1974). The program prompts the user to respond from a time-sharing terminal in a conversational format with the required input information. The program offers two major options: retrieval only; retrieval and plot. The first option retrieves mineral names, formulas, and groups from the file by identification number, by the mineral group code (a classification by chemistry or structure), or by searches based on the formula components. For example, it enables the user to search for minerals by major groups (i.e., feldspars, micas, amphiboles, oxides, phosphates, carbonates) by elemental composition (i.e., Fe, Cu, AI, Zn), or by a combination of these (i.e., all copper-bearing arsenates). The second option retrieves as the first, but also plots the retrieved 2-theta and intensity values as diagrammatic X-ray powder patterns on mylar sheets or overlays. These plots can be made using scale combinations compatible with chart recorder diffractograms and 114.59 mm powder camera films. The overlays are then used to separate or sieve out unrelated minerals until unknowns are matched and identified.

Neutron Diffraction and Electrical Transport Studies on Magnetic Transition in Terbium at High Pressures and Low Temperatures

NASA Astrophysics Data System (ADS)

Thomas, Sarah; Montgomery, Jeffrey; Tsoi, Georgiy; Vohra, Yogesh; Weir, Samuel; Tulk, Christopher; Moreira Dos Santos, Antonio

2013-06-01

Neutron diffraction and electrical transport measurements have been carried out on the heavy rare earth metal terbium at high pressures and low temperatures in order to elucidate its transition from a helical antiferromagnetic to a ferromagnetic ordered phase as a function of pressure. The electrical resistance measurements using designer diamonds show a change in slope as the temperature is lowered through the ferromagnetic Curie temperature. The temperature of the ferromagnetic transition decreases at a rate of -16.7 K/GPa till 3.6 GPa, where terbium undergoes a structural transition from hexagonal close packed (hcp) to an α-Sm phase. Above this pressure, the electrical resistance measurements no longer exhibit a change in slope. In order to confirm the change in magnetic phase suggested by the electrical resistance measurements, neutron diffraction measurements were conducted at the SNAP beamline at the Oak Ridge National Laboratory. Measurements were made at pressures to 5.3 GPa and temperatures as low as 90 K. An abrupt increase in peak intensity in the neutron diffraction spectra signaled the onset of magnetic order below the Curie temperature. A magnetic phase diagram of rare earth metal terbium will be presented to 5.3 GPa and 90 K based on these studies.

Characterisation of spray dried soy sauce powders made by adding crystalline carbohydrates to drying carrier.

PubMed

Wang, Wei; Zhou, Weibiao

2015-02-01

This study aimed to reduce stickiness and caking of spray dried soy sauce powders by introducing a new crystalline structure into powder particles. To perform this task, soy sauce powders were formulated by using mixtures of cellulose and maltodextrin or mixtures of waxy starch and maltodextrin as drying carriers, with a fixed carrier addition rate of 30% (w/v) in the feed solution. The microstructure, crystallinity, solubility as well as stickiness and caking strength of all the different powders were analysed and compared. Incorporating crystalline carbohydrates in the drying carrier could significantly reduce the stickiness and caking strength of the powders when the ratio of crystalline carbohydrates to maltodextrin was above 1:5 and 1:2, respectively. X-ray Diffraction (XRD) results showed that adding cellulose or waxy starch could induce the crystallinity of powders. Differential Scanning Calorimetry (DSC) results demonstrated that the native starch added to the soy sauce powders did not fully gelatinize during spray drying. Copyright © 2014 Elsevier Ltd. All rights reserved.

Cation ordering/disordering kinetics in Ba3CoNb2O9: An in situ study using synchrotron x-ray powder diffraction

NASA Astrophysics Data System (ADS)

Mallinson, P. M.; Claridge, J. B.; Rosseinsky, M. J.; Ibberson, R. M.; Wright, J. P.; Fitch, A. N.; Price, T.; Iddles, D. M.

2007-11-01

In situ synchrotron x-ray powder diffraction has been used to study the kinetics of cation ordering and disordering in the microwave dielectric electroceramic Ba3CoNb2O9 with a time resolution of 15s. The method enables the order/disorder temperature (To /d) in this material of 1430°C to be directly observed. The changes in the rate and degree of cation ordering and in the growth of ordered domains between samples ordered from standard precursor material and then subsequently reordered following an annealing period above To /d show that small changes in precursor order state and phase assemblage strongly influence the final domain size.

Comparison Study on Additive Manufacturing (AM) and Powder Metallurgy (PM) AlSi10Mg Alloys

NASA Astrophysics Data System (ADS)

Chen, B.; Moon, S. K.; Yao, X.; Bi, G.; Shen, J.; Umeda, J.; Kondoh, K.

2018-02-01

The microstructural and mechanical properties of AlSi10Mg alloys fabricated by additive manufacturing (AM) and powder metallurgy (PM) routes were investigated and compared. The microstructures were examined by scanning electron microscopy assisted with electron-dispersive spectroscopy. The crystalline features were studied by x-ray diffraction and electron backscatter diffraction. Room-temperature tensile tests and Vickers hardness measurements were performed to characterize the mechanical properties. It was found that the AM alloy had coarser Al grains but much finer Si precipitates compared with the PM alloy. Consequently, the AM alloy showed more than 100% increment in strength and hardness compared with the PM alloy due to the presence of ultrafine forms of Si, while exhibiting moderate ductility.

Growth and properties of benzil doped benzimidazole (BMZ) single crystals

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

Babu, R. Ramesh, E-mail: rampap2k@yahoo.co.in; Crystal Growth and Crystallography Section, National Physical Laboratory, Krishnan Marg, New Delhi 110 012; Sukumar, M.

2010-09-15

In the present work, we have made an attempt to study the effect of benzil doping on the properties of benzimidazole single crystals. For this purpose we have grown pure and benzil doped benzimidazole single crystals by vertical Bridgman technique. The grown crystals were characterized by various characterization techniques. The presence of dopants confirmed by powder X-ray diffraction (XRD). Crystalline perfection of the grown crystals has been analysed by high-resolution X-ray diffraction (HRXRD). The transmittance, electrical property and mechanical strength have been analysed using UV-vis-NIR spectroscopic, dielectric and Vicker's hardness studies. The relative second harmonic generation efficiency of pure andmore » doped benzimidazole crystals measured using Kurtz powder test.« less

Asymmetric band flipping for time-of-flight neutron diffraction data

DOE PAGES

Whitfield, Pamela S.; Coelho, Alan A.

2016-08-24

Charge flipping with powder diffraction data is known to produce a result more reliably with high-resolution data,i.e.visible reflections at smalldspacings. This data are readily accessible with the neutron time-of-flight technique but the assumption that negative scattering density is nonphysical is no longer valid where elements with negative scattering lengths are present. The concept of band flipping was introduced in the literature, where a negative threshold is used in addition to a positive threshold during the flipping. But, it was not tested with experimental data at the time. Finallly, band flipping has been implemented inTOPAStogether with the band modification of low-densitymore » elimination and tested with experimental powder and Laue single-crystal neutron data.« less

Magnetic and neutron diffraction study on quaternary oxides MTeMoO6 (M = Mn and Zn)

NASA Astrophysics Data System (ADS)

Doi, Yoshihiro; Suzuki, Ryo; Hinatsu, Yukio; Ohoyama, Kenji

2009-01-01

Crystal structures and magnetic properties of quaternary oxides MTeMoO6 (M = Mn and Zn) were investigated. From the Rietveld analyses for the powder x-ray and neutron diffraction measurements, their detailed structures have been determined. Both compounds have orthorhombic structure with space group P 21212 and a charge configuration of M2+Te4+Mo6+O6. ZnTeMoO6 shows diamagnetic behavior. In this structure, M ions are arranged in a square-planar manner. The temperature dependence of the magnetic susceptibility for MnTeMoO6 shows a broad peak at ~33 K, which is due to a two-dimensional characteristic of the magnetic interaction. In addition, this compound shows an antiferromagnetic transition at 20 K. The magnetic structure was determined by the powder neutron diffraction measurement at 3.3 K. The magnetic moments of Mn2+ ions (4.45 μB) order in a collinear antiferromagnetic arrangement along the b axis.

Photocatalytic degradation of diethyl phthalate using TiO{sub 2} nanoparticles

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

Singla, Pooja, E-mail: pooja.singla@thapar.edu; Pandey, O. P., E-mail: pooja.singla@thapar.edu; Singh, K., E-mail: pooja.singla@thapar.edu

2014-04-24

TiO{sub 2} nanoparticles predominantly in rutile phase are synthesized by ultrasonication assisted sol-gel method. TiO{sub 2} powder is characterized using X-ray powder diffraction and UV-vis diffuse reflectance. TiO{sub 2} is used as catalyst in photocatalytic degradation of Diethyl Phthalate. TiO{sub 2} exhibits good photocatalytic activity for the degradation of diethyl phthalate.

Powder Handling Device for Analytical Instruments

NASA Technical Reports Server (NTRS)

Sarrazin, Philippe C. (Inventor); Blake, David F. (Inventor)

2006-01-01

Method and system for causing a powder sample in a sample holder to undergo at least one of three motions (vibration, rotation and translation) at a selected motion frequency in order to present several views of an individual grain of the sample. One or more measurements of diffraction, fluorescence, spectroscopic interaction, transmission, absorption and/or reflection can be made on the sample, using light in a selected wavelength region.

Characterization of powdered fish heads for bone graft biomaterial applications.

PubMed

Oteyaka, Mustafa Ozgür; Unal, Hasan Hüseyin; Bilici, Namık; Taşçı, Eda

2013-01-01

The aim of this study was to define the chemical composition, morphology and crystallography of powdered fish heads of the species Argyrosomus regius for bone graft biomaterial applications. Two sizes of powder were prepared by different grinding methods; Powder A (coarse, d50=68.5 µm) and Powder B (fine, d50=19.1 µm). Samples were analyzed using X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), thermogravimetry (TG), and energy dispersive X-ray spectroscopy (EDS). The powder was mainly composed of aragonite (CaCO3) and calcite (CaCO3). The XRD pattern of Powder A and B matched standard aragonite and calcite patterns. In addition, the calcium oxide (CaO) phase was found after the calcination of Powder A. Thermogravimetry analysis confirmed total mass losses of 43.6% and 47.3% in Powders A and B, respectively. The microstructure of Powder A was mainly composed of different sizes and tubular shape, whereas Powder B showed agglomerated particles. The high quantity of CaO and other oxides resemble the chemical composition of bone. In general, the powder can be considered as bone graft after transformation to hydroxyapatite phase.

Microfocusing of the FERMI@Elettra FEL beam with a K-B active optics system: Spot size predictions by application of the WISE code

NASA Astrophysics Data System (ADS)

Raimondi, L.; Svetina, C.; Mahne, N.; Cocco, D.; Abrami, A.; De Marco, M.; Fava, C.; Gerusina, S.; Gobessi, R.; Capotondi, F.; Pedersoli, E.; Kiskinova, M.; De Ninno, G.; Zeitoun, P.; Dovillaire, G.; Lambert, G.; Boutu, W.; Merdji, H.; Gonzalez, A. I.; Gauthier, D.; Zangrando, M.

2013-05-01

FERMI@Elettra, the first seeded EUV-SXR free electron laser (FEL) facility located at Elettra Sincrotrone Trieste has been conceived to provide very short (10-100 fs) pulses with ultrahigh peak brightness and wavelengths from 100 nm to 4 nm. A section fully dedicated to the photon transport and analysis diagnostics, named PADReS, has already been installed and commissioned. Three of the beamlines, EIS-TIMEX, DiProI and LDM, installed after the PADReS section, are in advanced commissioning state and will accept the first users in December 2012. These beam lines employ active X-ray optics in order to focus the FEL beam as well as to perform a controlled beam-shaping at focus. Starting from mirror surface metrology characterization, it is difficult to predict the focal spot shape applying only methods based on geometrical optics such as the ray tracing. Within the geometrical optics approach one cannot take into account the diffraction effect from the optics edges, i.e. the aperture diffraction, and the impact of different surface spatial wavelengths to the spot size degradation. Both these effects are strongly dependent on the photon beam energy and mirror incident angles. We employed a method based on physical optics, which applies the Huygens-Fresnel principle to reflection (on which the WISE code is based). In this work we report the results of the first measurements of the focal spot in the DiProI beamline end-station and compare them to the predictions computed with Shadow code and WISE code, starting from the mirror surface profile characterization.

Light in the darkening on Naica gypsum crystals

NASA Astrophysics Data System (ADS)

Castillo-Sandoval, I.; Fuentes-Cobas, L. E.; Fuentes-Montero, M. E.; Esparza-Ponce, H. E.; Carreno-Márquez, J.; Reyes-Cortes, M.; Montero-Cabrera, M. E.

2015-07-01

Naica mine is located in a semi-desertic region at the central-south of Chihuahua State. The Cave of Swords was discovered in 1910 and the Cave of Crystals 90 years later at Naica mines. It is expected that during the last century the human presence has changed the microclimatic conditions inside the cave, resulting in the deterioration of the crystals and the deposition of impurities on gypsum surfaces. As a contribution to the clarification of the mentioned issues, the present work refers to the use of synchrotron radiation for the identification of phases on these surfaces. All the experiments were performed at the Stanford Synchrotron Radiation Lightsource. Grazing incidence X-ray diffraction (GIXRD) and radiography-aided X-ray diffraction (RAXRD) experiments were performed at beamline 11-3. X-Ray micro-fluorescence (μ-SXRF) and micro-X-ray absorption (μ-XANES) were measured at beamline 2-3. Representative results obtained may be summarized as follows: a) Gypsum, galena, sphalerite, hematite and cuprite at the surface of the gypsum crystals were determined. b) The samples micro-structure is affected by impurities. c) The elemental distributions and correlations (0.6-0.9) of Cu, K, Fe, Mn, Pb, Zn, Ca and S were identified by μ-SXRF. The correlations among elemental contents confirmed the phase identification, with the exception of manganese and potassium due to the amorphous nature of some impurity compounds in these samples. The compounds hematite (Fe2O3), β-MnO2, Mn2O3, MnO and/or MnCO3, PbS, PbCO3 and/or PbSO4, ZnO4, ZnS and/or smithsonite (ZnCO3), CuS + Cu Oxide were identified by XANES. Plausibly, these latter compounds do not form crystalline phases.

Mutual optical intensity propagation through non-ideal mirrors

DOE PAGES

Meng, Xiangyu; Shi, Xianbo; Wang, Yong; ...

2017-08-18

The mutual optical intensity (MOI) model is extended to include the propagation of partially coherent radiation through non-ideal mirrors. The propagation of the MOI from the incident to the exit plane of the mirror is realised by local ray tracing. The effects of figure errors can be expressed as phase shifts obtained by either the phase projection approach or the direct path length method. Using the MOI model, the effects of figure errors are studied for diffraction-limited cases using elliptical cylinder mirrors. Figure errors with low spatial frequencies can vary the intensity distribution, redistribute the local coherence function and distortmore » the wavefront, but have no effect on the global degree of coherence. The MOI model is benchmarked againstHYBRIDand the multi-electronSynchrotron Radiation Workshop(SRW) code. The results show that the MOI model gives accurate results under different coherence conditions of the beam. Other than intensity profiles, the MOI model can also provide the wavefront and the local coherence function at any location along the beamline. The capability of tuning the trade-off between accuracy and efficiency makes the MOI model an ideal tool for beamline design and optimization.« less

Fully Automated Data Collection Using PAM and the Development of PAM/SPACE Reversible Cassettes

NASA Astrophysics Data System (ADS)

Hiraki, Masahiko; Watanabe, Shokei; Chavas, Leonard M. G.; Yamada, Yusuke; Matsugaki, Naohiro; Igarashi, Noriyuki; Wakatsuki, Soichi; Fujihashi, Masahiro; Miki, Kunio; Baba, Seiki; Ueno, Go; Yamamoto, Masaki; Suzuki, Mamoru; Nakagawa, Atsushi; Watanabe, Nobuhisa; Tanaka, Isao

2010-06-01

To remotely control and automatically collect data in high-throughput X-ray data collection experiments, the Structural Biology Research Center at the Photon Factory (PF) developed and installed sample exchange robots PAM (PF Automated Mounting system) at PF macromolecular crystallography beamlines; BL-5A, BL-17A, AR-NW12A and AR-NE3A. We developed and installed software that manages the flow of the automated X-ray experiments; sample exchanges, loop-centering and X-ray diffraction data collection. The fully automated data collection function has been available since February 2009. To identify sample cassettes, PAM employs a two-dimensional bar code reader. New beamlines, BL-1A at the Photon Factory and BL32XU at SPring-8, are currently under construction as part of Targeted Proteins Research Program (TPRP) by the Ministry of Education, Culture, Sports, Science and Technology of Japan. However, different robots, PAM and SPACE (SPring-8 Precise Automatic Cryo-sample Exchanger), will be installed at BL-1A and BL32XU, respectively. For the convenience of the users of both facilities, pins and cassettes for PAM and SPACE are developed as part of the TPRP.

Single-crystal diffraction at the Extreme Conditions beamline P02.2: procedure for collecting and analyzing high-pressure single-crystal data.

PubMed

Rothkirch, André; Gatta, G Diego; Meyer, Mathias; Merkel, Sébastien; Merlini, Marco; Liermann, Hanns Peter

2013-09-01

Fast detectors employed at third-generation synchrotrons have reduced collection times significantly and require the optimization of commercial as well as customized software packages for data reduction and analysis. In this paper a procedure to collect, process and analyze single-crystal data sets collected at high pressure at the Extreme Conditions beamline (P02.2) at PETRA III, DESY, is presented. A new data image format called `Esperanto' is introduced that is supported by the commercial software package CrysAlis(Pro) (Agilent Technologies UK Ltd). The new format acts as a vehicle to transform the most common area-detector data formats via a translator software. Such a conversion tool has been developed and converts tiff data collected on a Perkin Elmer detector, as well as data collected on a MAR345/555, to be imported into the CrysAlis(Pro) software. In order to demonstrate the validity of the new approach, a complete structure refinement of boron-mullite (Al5BO9) collected at a pressure of 19.4 (2) GPa is presented. Details pertaining to the data collections and refinements of B-mullite are presented.

The effect of polymorphism on powder compaction and dissolution properties of chemically equivalent oxytetracycline hydrochloride powders.

PubMed

Liebenberg, W; de Villiers, M M; Wurster, D E; Swanepoel, E; Dekker, T G; Lötter, A P

1999-09-01

In South Africa, oxytetracycline is identified as an essential drug; many generic products are on the market, and many more are being developed. In this study, six oxytetracycline hydrochloride powders were obtained randomly from manufacturers, and suppliers were compared. It was found that compliance to a pharmacopoeial monograph was insufficient to ensure the optimum dissolution performance of a simple tablet formulation. Comparative physicochemical raw material analysis showed no major differences with regard to differential scanning calorimetry (DSC), infrared (IR) spectroscopy, powder dissolution, and particle size. However, the samples could be divided into two distinct types with respect to X-ray powder diffraction (XRD) and thus polymorphism. The two polymorphic forms had different dissolution properties in water or 0.1 N hydrochloride acid. This difference became substantial when the dissolution from tablets was compared. The powders containing form A were less soluble than that containing form B.

Aqueous Combustion Synthesis and Characterization of Nanosized Tetragonal Zirconia Single Crystals

NASA Astrophysics Data System (ADS)

Reddy, B. S. B.; Mal, Indrajit; Tewari, Shanideep; Das, Karabi; Das, Siddhartha

2007-08-01

Nanocrystalline zirconia powder has been synthesized by an aqueous combustion synthesis route using glycine as fuel and nitrate as oxidizer. The powders have been prepared by using different glycine to zirconyl nitrate molar ratios (G/N). The powders produced with different G/N ratios have been characterized by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) to determine the parameters resulting from powder with attractive properties. The theoretical combustion temperature (T ad ) has been calculated for different G/N ratios, and it is correlated with powder characteristics. An attempt is also made to explain the stability of tetragonal zirconia on the basis of extrinsic factors such as the morphology of nanocrystallites. Nanocrystalline metastable tetragonal zirconia (˜25 nm) powder (TZ) with disc-shaped morphology has been produced with a weak agglomeration in fuel deficient mixtures.

Rietveld analysis of X-ray powder diffraction patterns as a potential tool for the identification of impact-deformed carbonate rocks

NASA Astrophysics Data System (ADS)

Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

2009-12-01

Previous X-ray powder diffraction (XRD) studies revealed that shock deformed carbonates and quartz have broader XRD patterns than those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas, unshocked equivalent samples from 95 miles north of the crater and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a potential tool for distinguishing impact deformed rocks from unshocked and tectonically deformed rocks. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Unshocked equivalent dolostone samples were collected from well cores drilled outside of the impact crater. Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenic belts. Whereas calcite subjected to significant shock intensities at the Sierra Madera impact crater can be differentiated from tectonically deformed calcite from the Mission Canyon Formation using Rietveld refined peak profiles, weakly shocked calcite from the crater rim appears to be indistinguishable from the tectonically deformed calcite. In contrast, Rietveld analysis readily distinguishes shocked Sierra Madera dolomite from unshocked equivalent dolostone samples from outside the crater and tectonically deformed Mission Canyon Formation dolomite.

Evidence for weak ferromagnetism, isostructural phase transition, and linear magnetoelectric coupling in the multiferroic Bi0.8Pb0.2Fe0.9Nb0.1O3 solid solution

NASA Astrophysics Data System (ADS)

Patel, Jay Prakash; Senyshyn, Anatoliy; Fuess, Hartmut; Pandey, Dhananjai

2013-09-01

Magnetization, dielectric, and calorimetric studies on Bi0.8 Pb0.2 Fe0.9 Nb0.1O3 (BF-0.2PFN) reveal very weak ferromagnetism but strong dielectric anomaly at the antiferromagnetic transition temperature (TN) characteristic of magnetoelectric coupling. We correlate these results with nuclear and magnetic structure studies using x-ray and neutron powder diffraction techniques, respectively. Rietveld refinements using x-ray powder diffraction data in the temperature range 300 to 673 K reveal pronounced anomalies in the unit cell parameters at TN, indicating strong magnetoelastic coupling. The nuclear and magnetic structures of BF-0.2PFN were determined from neutron powder diffraction data using a representation theory approach. They show the occurrence of a first-order isostructural phase transition (IPT) accompanying the magnetic ordering below TN˜566 K, leading to significant discontinuous change in the ionic polarization (ΔPz˜1.6(3) μC/cm2) and octahedral tilt angle (˜0.3°) at TN. The ionic polarization obtained from refined positional coordinates of the nuclear structure and Born effective charges is shown to scale linearly with sublattice magnetization, confirming the presence of linear magnetoelectric coupling in BF-0.2PFN at the atomic level, despite the very low value of remanent magnetization (Mr).

The Advanced Light Source (ALS) Slicing Undulator Beamline

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

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

2007-01-19

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

Effect of titanium on the structural and optical property of NiO nano powders

NASA Astrophysics Data System (ADS)

Amin, Ruhul; Mishra, Prashant; Khatun, Nasima; Ayaz, Saniya; Srivastava, Tulika; Sen, Somaditya

2018-05-01

Nickel Oxide (NiO) and Ti doped NiO nanoparticles were prepared by sol-gel auto combustion method. Powder x-ray diffraction (PXRD) structural studies revealed face centered cubic (FCC) structure of the NiO nanopowders. The crystallite size decreased with Ti incorporation. UV-Vis spectroscopy carried out in diffused reflectance mode revealed decrease in band gap with increment in Urbach energy with doping.

Flexible graphene composites for removal of methylene blue dye-contaminant from water

NASA Astrophysics Data System (ADS)

Oliva, J.; Martinez, A. I.; Oliva, A. I.; Garcia, C. R.; Martinez-Luevanos, A.; Garcia-Lobato, M.; Ochoa-Valiente, R.; Berlanga, A.

2018-04-01

This work presents the use of flexible graphene composites (FGCs) fabricated by a casting method for the removal of Methylene blue (MB) dye from water. Those FGCs with elastic modulus of 15 MPa had enough mechanical resistance to support the Al2O3:Eu3+ and SrAl2O4:Bi3+ photocatalytic powders. After the incorporation of those powders in the FGCs, their photocatalytic activity was evaluated by monitoring the degradation of MB dye under solar irradiation. Scanning electron microscopy (SEM) images demonstrate that the surface of FGCs with catalysts powders presents pores with sizes in the range of 15-40 μm, which favored the sunlight absorption by scattering effects. Moreover, X-Ray diffraction measurements confirmed the formation of the composites by displacements of their diffraction peaks. The MB dye was completely removed (by photocatalysis and by physical adsorption) from the water after 180 min and 270 min by using the FGCs with Al2O3:Eu3+ and SrAl2O4:Bi3+ catalysts respectively. Hence, the results of photocatalytic activity suggest that our FGCs could be used as an effective support of catalyst powders for the easy removal of dye contaminants in wastewater treatment plants.

Extraction of Lithium from Brine Solution by Hydrolysis of Activated Aluminum Powder

NASA Astrophysics Data System (ADS)

Li, Yanhong; Chen, Xingyu; Liu, Xuheng; Zhao, Zhongwei; Liu, Chongwu

2018-05-01

Activated aluminum powder has been used to extract lithium from Mg-Li mixed solution via a hydrolysis-adsorption reaction. First, activated aluminum powder was prepared under the optimal conditions of NaCl addition of 70%, ball-milling time of 3 h, and ball-to-powder mass ratio of 20:1. Then, the activated aluminum powder was added into the Mg-Li mixed solution to extract lithium. X-ray diffraction analysis indicated that Li+ was adsorbed by freshly formed Al(OH)3 in the form of LADH-Cl [LiCl·2Al(OH)3·mH2O]. Under the optimal conditions of reaction time of 3 h, Al/Li molar ratio of 4:1 for activated aluminum powder addition, and reaction temperature of 70°C, lithium precipitation exceeded 90% while magnesium precipitation was controlled at 13%. These results indicate that activated aluminum powder can efficiently extract lithium from Mg-Li mixed solution via a hydrolysis-adsorption reaction.

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

Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de

A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ballmore » milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.« less

Characterization of monoclinic crystals in tablets by pattern-fitting procedure using X-ray powder diffraction data.

PubMed

Yamamura, Shigeo; Momose, Yasunori

2003-06-18

The purpose of this study is to characterize the monoclinic crystals in tablets by using X-ray powder diffraction data and to evaluate the deformation feature of crystals during compression. The monoclinic crystals of acetaminophen and benzoic acid were used as the samples. The observed X-ray diffraction intensities were fitted to the analytic expression, and the fitting parameters, such as the lattice parameters, the peak-width parameters, the preferred orientation parameter and peak asymmetric parameter were optimized by a non-linear least-squares procedure. The Gauss and March distribution functions were used to correct the preferred orientation of crystallites in the tablet. The March function performed better in correcting the modification of diffraction intensity by preferred orientation of crystallites, suggesting that the crystallites in the tablets had fiber texture with axial orientation. Although a broadening of diffraction peaks was observed in acetaminophen tablets with an increase of compression pressure, little broadening was observed in the benzoic tablets. These results suggest that "acetaminophen is a material consolidating by fragmentation of crystalline particles and benzoic acid is a material consolidating by plastic deformation then occurred rearrangement of molecules during compression". A pattern-fitting procedure is the superior method for characterizing the crystalline drugs of monoclinic crystals in the tablets, as well as orthorhombic isoniazid and mannitol crystals reported in the previous paper.

Utilization of fish bone as adsorbent of Fe3+ ion by controllable removal of its carbonaceous component

NASA Astrophysics Data System (ADS)

Nurhadi, M.; Kusumawardani, R.; Widiyowati, I. I.; Wirhanuddin; Nur, H.

2018-05-01

The performance of fish bone to adsorb Fe3+ ion in solution was studied. Powdered fish bone and carbonized fish bone were used as adsorbent. All absorbents were characterized by X-ray diffraction (XRD), IR spectroscopy, nitrogen adsorption, scanning electron microscopy (SEM) and TG analysis. Powdered fish bone and carbonized fish bone were effective as adsorbent for removing Fe3+ ion in solution. The metal adsorptions of Fe3+ ion were 94 and 98% for powdered fish bone and fish bone which carbonized at 400 and 500 °C.

Relative impact of H 2 O and O 2 in the oxidation of UO 2 powders from 50 to 300 °C

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

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong

Here, we studied the reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO 2) powder at elevated temperature by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). We observed and quatified oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Relative impact of H2O and O2 in the oxidation of UO2 powders from 50 to 300 °C

NASA Astrophysics Data System (ADS)

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong; Roberts, Sarah K.; Nelson, Art J.

2017-12-01

The reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO2) powder at elevated temperature was studied by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). Oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice was observed and quantified. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Relative impact of H 2 O and O 2 in the oxidation of UO 2 powders from 50 to 300 °C

DOE PAGES

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong; ...

2017-10-04

Here, we studied the reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO 2) powder at elevated temperature by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). We observed and quatified oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Order-disorder-reorder process in thermally treated dolomite samples: a combined powder and single-crystal X-ray diffraction study

NASA Astrophysics Data System (ADS)

Zucchini, A.; Comodi, P.; Katerinopoulou, A.; Balic-Zunic, T.; McCammon, C.; Frondini, F.

2012-04-01

A combined powder and single-crystal X-ray diffraction analysis of dolomite [CaMg(CO3)2] heated to 1,200°C at 3 GPa was made to study the order-disorder-reorder process. The order/disorder transition is inferred to start below 1,100°C, and complete disorder is attained at approximately 1,200°C. Twinned crystals characterized by high internal order were found in samples annealed over 1,100°C, and their fraction was found to increase with temperature. Evidences of twinning domains combined with probable remaining disordered portions of the structure imply that reordering processes occur during the quench. Twin domains are hereby proposed as a witness to thermally induced intra-layer-type cation disordering.

Perylene and Perylene-Derivative Nano-Cocrystals: Preparation and Physicochemical Property

NASA Astrophysics Data System (ADS)

Baba, Koichi; Konta, Sayaka; Oliveira, Daniel; Sugai, Kenji; Onodera, Tsunenobu; Masuhara, Akito; Kasai, Hitoshi; Oikawa, Hidetoshi; Nakanishi, Hachiro

2012-12-01

Organic nano-cocrystals of functional dyes of perylene and a perylene derivative were successfully prepared by the reprecipitation method. The particle sizes, optical properties, and powder X-ray diffraction patterns of nano-cocrystals were evaluated. Typically, the size with size distribution of nano-cocrystals was 55±15 nm when the molar ratio of perylene to the perylene derivative was 50:50. The particular intermolecular electronic interaction between perylene and the perylene derivative in the nano-cocrystal state was observed by absorption and fluorescence spectra measurements. The powder X-ray diffraction pattern analysis confirmed that the structure of nano-cocrystals was different from those prepared from perylene and the perylene derivative. The nano-cocrystal having unique physicochemical properties will be potentially classified as a new type of functional nanomaterial.

Suppression of the commensurate magnetic phase in nanosized hübnerite MnW O 4

DOE PAGES

Zajdel, P.; G?gor, A.; Pajerowski, D. M.; ...

2017-05-18

Magnetic structures of nanosized (20 to 70 nm) powders of MnWO 4 and MnWO 4:Mo were studied using neutron powder diffraction (NPD). Sizes and shapes of the crystallites calculated from anisotropic peak broadening of diffraction peaks were found to be orthogonal parallelepipedlike with the longest edge along the c axis and the shortest along the b axis. SQUID measurements indicate the presence of two magnetic transitions around 8 and 12 K. Rietveld refinement of the NPD data below the magnetic transition was consistent with the presence of an incommensurate spiral-like (ac-AF2) phase. Finally, a commensurate phase AF1 was not observedmore » down to 2.5 K for all of the samples.« less

X-ray diffraction-based electronic structure calculations and experimental x-ray analysis for medical and materials applications

NASA Astrophysics Data System (ADS)

Mahato, Dip Narayan

This thesis includes x-ray experiments for medical and materials applications and the use of x-ray diffraction data in a first-principles study of electronic structures and hyperfine properties of chemical and biological systems. Polycapillary focusing lenses were used to collect divergent x rays emitted from conventional x-ray tubes and redirect them to form an intense focused beam. These lenses are routinely used in microbeam x-ray fluorescence analysis. In this thesis, their potential application to powder diffraction and focused beam orthovoltage cancer therapy has been investigated. In conventional x-ray therapy, very high energy (˜ MeV) beams are used, partly to reduce the skin dose. For any divergent beam, the dose is necessarily highest at the entry point, and decays exponentially into the tissue. To reduce the skin dose, high energy beams, which have long absorption lengths, are employed, and rotated about the patient to enter from different angles. This necessitates large expensive specialized equipment. A focused beam could concentrate the dose within the patient. Since this is inherently skin dose sparing, lower energy photons could be employed. A primary concern in applying focused beams to therapy is whether the focus would be maintained despite Compton scattering within the tissue. To investigate this, transmission and focal spot sizes as a function of photon energy of two polycapillary focusing lenses were measured. The effects of tissue-equivalent phantoms of different thicknesses on the focal spot size were studied. Scatter fraction and depth dose were calculated. For powder diffraction, the polycapillary optics provide clean Gaussian peaks, which result in angular resolution that is much smaller than the peak width due to the beam convergence. Powder diffraction (also called coherent scatter) without optics can also be used to distinguish between tissue types that, because they have different nanoscale structures, scatter at different angles. Measurements were performed on the development of coherent scatter imaging to provide tissue type information in mammography. Atomic coordinates from x-ray diffraction data were used to study the nuclear quadrupole interactions and nature of molecular binding in DNA/RNA nucleobases and molecular solid BF3 systems.

Rotary Valve & Beamline Highlights for Fiscal Year 2017

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

Fitsos, P

This Fiscal Year (FY) work was divided between continued testing and characterization work of the Rotary Valve (RV) and mechanical engineering support for the beamline hardware stands. This configuration is more like the final setup with the accelerator firing deuterons down the evacuated beamline toward the RV for interaction with the deuterium and neutron production. The beamline cells were part of an experiment to reduce the impact that RV gas would have on the beamline vacuum. This work will be reported separately from this report. Previous testing had been with the beamline at atmospheric pressure and now the goal wasmore » to get test results of the RV with it connected to a beamline that’s running at some level of vacuum.« less

Investigation of phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) by in situ synchrotron high-temperature powder diffraction

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

Ouyang, Xin; Huang, Saifang; School of Materials Science and Technology, China University of Geosciences

2014-03-15

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) precursors prepared via solid-state and sol–gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol–gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol–gel precursor. Both precursors are able to bemore » calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study. -- Graphical abstract: The in situ synchrotron HT-XRD patterns of CCTO sol–gel and solid-state precursor. Highlights: • Phase formation sequence/mechanism in two CCTO precursors has been established. • Formation temperature of CCTO via sol–gel method is lower than solid-state method. • Intermediate phases are only observed in the sol–gel precursor. • Both precursors are able to be calcined into sub-micrometric sized powders.« less

Some aspects of SR beamline alignment

NASA Astrophysics Data System (ADS)

Gaponov, Yu. A.; Cerenius, Y.; Nygaard, J.; Ursby, T.; Larsson, K.

2011-09-01

Based on the Synchrotron Radiation (SR) beamline optical element-by-element alignment with analysis of the alignment results an optimized beamline alignment algorithm has been designed and developed. The alignment procedures have been designed and developed for the MAX-lab I911-4 fixed energy beamline. It has been shown that the intermediate information received during the monochromator alignment stage can be used for the correction of both monochromator and mirror without the next stages of alignment of mirror, slits, sample holder, etc. Such an optimization of the beamline alignment procedures decreases the time necessary for the alignment and becomes useful and helpful in the case of any instability of the beamline optical elements, storage ring electron orbit or the wiggler insertion device, which could result in the instability of angular and positional parameters of the SR beam. A general purpose software package for manual, semi-automatic and automatic SR beamline alignment has been designed and developed using the developed algorithm. The TANGO control system is used as the middle-ware between the stand-alone beamline control applications BLTools, BPMonitor and the beamline equipment.

From Soft to Hard X-ray with a Single Grating Monochromator

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

Cocco, D.; Bianco, A.; Kaulich, B.

Even if not well defined a border exists between the soft and the hard X-ray region. The optics adopted in one region is not suitable for the other region and vice versa. Nevertheless, recently more and more experimentalists wish to investigate their samples by using an energy range as wide as possible. Without adopting complicated and very expensive mechanical solutions, it is a major challenge, for the optical designer, to find a solution suitable for both spectral ranges. This was our task for the TwinMic beamline at Elettra, the Italian 3rd generation synchrotron radiation source. This beamline will house amore » twin x-ray microscope, which combines scanning and full-field imaging in a single multipurpose end station and is operated in the 0.2-3 keV photon energy range. This energy range will be covered by a blazed grating, which has a very shallow blaze angle of 0.4 deg. With this grating mechanically ruled in the grating laboratory of Carl Zeiss very high diffraction efficiency can be achieved, expected to be higher then 10% over the whole range. This grating was tested at the KMC 1 beamline in BESSY, which is particularly suitable for this kind of measurements since it has a crystal monochromator that can go down to 1.7 keV and can be equipped with an high precision diffractometer. The obtained results demonstrate that it is possible to work with this grating up to 6 keV with still enough efficiency (5% at 6 keV and 15% at 1.8 keV). The efficiency in the lower part of the energy range was tested at Elettra, again with very good results (more then 20% at 950 eV and 15% at 600eV). A second grating, also produced by Carl Zeiss, with a blaze angle of 1.1 deg. will be mounted in the same monochromator, to cover the lower energy range. Both gratings have 600 grooves/mm, which is a good compromise for achieving the requested energy resolving power (of the order of 4000 in most of the range) and to have as much flux as possible, mandatory for the experiments proposed for this beamline. A multilayer mirror, mounted side by side with the two gratings, will permit a wide band selection of the incoming radiation. The beamline is expected to be operative in spring 2007.« less

Evidence for existence of functional monoclinic phase in sodium niobate based solid solution by powder neutron diffraction

NASA Astrophysics Data System (ADS)

Mishra, S. K.; Jauhari, Mrinal; Mittal, R.; Krishna, P. S. R.; Reddy, V. R.; Chaplot, S. L.

2018-04-01

We have carried out systematic temperature-dependent neutron diffraction measurements in conjunction with dielectric spectroscopy from 6 to 300 K for sodium niobate based compounds (1-x) NaNbO3-xBaTiO3 (NNBTx). The dielectric constant is measured as a function of both temperature and frequency. It shows an anomaly at different temperatures in cooling and heating cycles and exhibits a large thermal hysteresis of ˜150 K for the composition x = 0.03. The dielectric constant is found to be dispersive in nature and suggests a relaxor ferroelectric behavior. In order to explore structural changes as a function of temperature, we analyzed the powder neutron diffraction data for the compositions x = 0.03 and 0.05. Drastic changes are observed in the powder profiles near 2θ ˜ 30.6°, 32.1°, and 34.6° in the diffraction pattern below 200 K during cooling and above 190 K in heating cycles, respectively. The disappearance of superlattice reflection and splitting in main perovskite peaks provide a signature for structural phase transition. We observed stabilization of a monoclinic phase (Cc) at low temperature. This monoclinic phase is believed to provide a flexible polarization rotation and considered to be directly linked to the high performance piezoelectricity in materials. The thermal hysteresis for composition x = 0.03 is larger than that for x = 0.05. This suggests that the addition of BaTiO3 to NaNbO3 suppresses the thermal hysteresis. It is also observed that the structural phase transition temperature decreases upon increasing the dopant concentration.

Macroscopic X-ray Powder Diffraction Scanning: Possibilities for Quantitative and Depth-Selective Parchment Analysis.

PubMed

Vanmeert, Frederik; De Nolf, Wout; Dik, Joris; Janssens, Koen

2018-06-05

At or below the surface of painted works of art, valuable information is present that provides insights into an object's past, such as the artist's technique and the creative process that was followed or its conservation history but also on its current state of preservation. Various noninvasive techniques have been developed over the past 2 decades that can probe this information either locally (via point analysis) or on a macroscopic scale (e.g., full-field imaging and raster scanning). Recently macroscopic X-ray powder diffraction (MA-XRPD) mapping using laboratory X-ray sources was developed. This method can visualize highly specific chemical distributions at the macroscale (dm 2 ). In this work we demonstrate the synergy between the quantitative aspects of powder diffraction and the noninvasive scanning capability of MA-XRPD highlighting the potential of the method to reveal new types of information. Quantitative data derived from a 15th/16th century illuminated sheet of parchment revealed three lead white pigments with different hydrocerussite-cerussite compositions in specific pictorial elements, while quantification analysis of impurities in the blue azurite pigment revealed two distinct azurite types: one rich in barite and one in quartz. Furthermore, on the same artifact, the depth-selective possibilities of the method that stem from an exploitation of the shift of the measured diffraction peaks with respect to reference data are highlighted. The influence of different experimental parameters on the depth-selective analysis results is briefly discussed. Promising stratigraphic information could be obtained, even though the analysis is hampered by not completely understood variations in the unit cell dimensions of the crystalline pigment phases.

M(II)-dipyridylamide-based coordination frameworks (M=Mn, Co, Ni): Structural transformation

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

Tzeng, Biing-Chiau; Selvam, TamilSelvi; Tsai, Miao-Hsin

2016-11-15

A series of 1-D double-zigzag (([M(papx){sub 2}(H{sub 2}O){sub 2}](ClO{sub 4}){sub 2}){sub n}; M=Mn, x=s (1), x=o (3); M=Co, x=s (4), x=o (5); M=Ni, x=s (6), x=o (7)) and 2-D polyrotaxane ([Mn(paps){sub 2}(ClO{sub 4}){sub 2}]{sub n} (2)) frameworks were synthesized by reactions of M(ClO{sub 4}){sub 2} (M=Mn, Co, and Ni) with papx (paps, N,N’-bis(pyridylcarbonyl)-4,4’-diaminodiphenylthioether; papo, N,N’-bis(pyridylcarbonyl)-4,4’-diaminodiphenyl ether), which have been isolated and structurally characterized by X-ray diffraction. Based on powder X-ray diffraction (PXRD) experiments, heating the double-zigzag frameworks underwent structural transformation to give the respective polyrotaxane ones. Moreover, grinding the solid samples of the respective polyrotaxanes in the presence of moisturemore » also resulted in the total conversion to the original double-zigzag frameworks. In this study, we have successfully extended studies to Mn{sup II}, Co{sup II}, and Ni{sup II} frameworks from the previous Zn{sup II}, Cd{sup II}, and Cu{sup II} ones, and interestingly such structural transformation is able to be proven experimentally by powder and single-crystal X-ray diffraction studies as well. - Graphical abstract: 1-D double-zigzag and 2-D polyrotaxane frameworks of M(II)-papx (x=s, o; M=Mn, Co, Ni) frameworks can be interconverted by heating and grinding in the presence of moiture, and such structural transformation has be proven experimentally by powder and single-crystal X-ray diffraction studies.« less

Chemical Reduction of Nd 1.85 Ce 0.15 CuO 4− δ Powders in Supercritical Sodium Ammonia Solutions

DOE PAGES

Dias, Yasmin; Wang, Hui; Zhou, Haiqing; ...

2015-01-01

Nd 1.85 Ce 0.15 CuO 4− δ powders are chemically reduced in supercritical sodium ammonia solutions from room temperature to 350°C. The crystallographic structure of the reduced powders is investigated from Rietveld refinement of X-ray powder diffraction. The atomic positions are maintained constant within experimental errors while temperature factors of all atoms increase significantly after the chemical treatments, especially of Nd/Ce atoms. The ammonothermally reduced Nd 1.85 Ce 0.15 CuO 4− δ powders show diamagnetic below 24 K which is contributed to the lower oxygen content and higher temperature factors of atoms in the treated compound. Themore » ammonothermal method paves a new way to reduce oxides in supercritical solutions near room temperature.« less

Mechanical alloying, characterization and consolidation of Ti-Al-Ni alloys

NASA Technical Reports Server (NTRS)

Nash, P.; Higgins, G. T.; Dillinger, N.; Hwang, S. J.; Kim, H.

1989-01-01

Mechanical alloying is being investigated as a processing route for the production of aluminide intermetallics. This program involves powder production and characterization, consolidation and thermal treatments and determination of microstructure-property relationships. An attritor mill is being used to produce powder in lots up to 1000 grams and the processing parameters are being systematically varied to establish the optimum milling conditions. The mill is being instrumented to generate data related to the processing to provide a basis for theoretical modeling. Powder is being characterized using thermal analysis, optical and electron microscopy and X-ray diffraction. Particle size distributions and powder density are being determined. Consolidation of the powder is being approached in several different ways including, cold isostatic pressing, sintering, extrusion and hot pressing. The results of the program so far will be presented and future directions discussed.

Study of gold nanoparticle synthesis by synchrotron x-ray diffraction and fluorescence

NASA Astrophysics Data System (ADS)

Yan, Zhongying; Wang, Xiao; Yu, Le; Moeendarbari, Sina; Hao, Yaowu; Cai, Zhonghou; Cheng, Xuemei

Gold nanoparticles have a wide range of potential applications, including therapeutic agent delivery, catalysis, and electronics. Recently a new process of hollow nanoparticle synthesis was reported, the mechanism of which was hypothesized to involve electroless deposition around electrochemically evolved hydrogen bubbles. However, the growth mechanism still needs experimental evidence. We report investigation of this synthesis process using synchrotron x-ray diffraction and fluorescence measurements performed at beamline 2-ID-D of the Advanced Photon Source (APS). A series of gold nanoparticle samples with different synthesis time (50-1200 seconds) were deposited using a mixture electrolyte solution of Na3Au(SO3)2 and H4N2NiO6S2 on anodic aluminum oxide (AAO) membranes. The 2D mapping of fluorescence intensity and comparison of x-ray diffraction peaks of the samples have provided valuable information on the growth mechanism. Work at Bryn Mawr College and University of Texas at Arlington is supported by NSF Grants (1207085 and 1207377) and use of the APS at Argonne National Laboratory is supported by the U. S. Department of Energy under Contract No. DE-AC02-06CH11357.

Crystallization of Δ{sup 1}-tetrahydrocannabinolic acid (THCA) synthase from Cannabis sativa

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

Shoyama, Yoshinari; Takeuchi, Ayako; Taura, Futoshi

Δ{sup 1}-Tetrahydrocannabinolic acid (THCA) synthase from C. sativa was crystallized. The crystal diffracted to 2.7 Å resolution with sufficient quality for further structure determination. Δ{sup 1}-Tetrahydrocannabinolic acid (THCA) synthase is a novel oxidoreductase that catalyzes the biosynthesis of the psychoactive compound THCA in Cannabis sativa (Mexican strain). In order to investigate the structure–function relationship of THCA synthase, this enzyme was overproduced in insect cells, purified and finally crystallized in 0.1 M HEPES buffer pH 7.5 containing 1.4 M sodium citrate. A single crystal suitable for X-ray diffraction measurement was obtained in 0.09 M HEPES buffer pH 7.5 containing 1.26 Mmore » sodium citrate. The crystal diffracted to 2.7 Å resolution at beamline BL41XU, SPring-8. The crystal belonged to the primitive cubic space group P432, with unit-cell parameters a = b = c = 178.2 Å. The calculated Matthews coefficient was approximately 4.1 or 2.0 Å{sup 3} Da{sup −1} assuming the presence of one or two molecules of THCA synthase in the asymmetric unit, respectively.« less

Crystallization and preliminary X-ray diffraction analysis of hemextin A: a unique anticoagulant protein from Hemachatus haemachatus venom

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

Banerjee, Yajnavalka; Kumar, Sundramurthy; Jobichen, Chacko

2007-08-01

Crystals of hemextin A, a three-finger toxin isolated and purified from African Ringhals cobra (H. haemachatus), are orthorhombic, space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 49.27, b = 49.51, c = 57.87 Å, and diffract to 1.5 Å resolution. Hemextin A was isolated and purified from African Ringhals cobra (Hemachatus haemachatus). It is a three-finger toxin that specifically inhibits blood coagulation factor VIIa and clot formation and that also interacts with hemextin B to form a unique anticoagulant complex. Hemextin A was crystallized by the hanging-drop vapour-diffusion method by equilibration against 0.2 M ammonium acetate, 0.1more » M sodium acetate trihydrate pH 4.6 and 30% PEG 4000 as the precipitating agent. The crystals belong to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 49.27, b = 49.51, c = 57.87 Å and two molecules in the asymmetric unit. They diffracted to 1.5 Å resolution at beamline X25 at BNL.« less

Integrated nonlinear optical imaging microscope for on-axis crystal detection and centering at a synchrotron beamline

PubMed Central

Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.; Newman, Justin A.; Oglesbee, Robert A.; Hedderich, Hartmut G.; Everly, R. Michael; Becker, Michael; Ronau, Judith A.; Buchanan, Susan K.; Cherezov, Vadim; Morrow, Marie E.; Xu, Shenglan; Ferguson, Dale; Makarov, Oleg; Das, Chittaranjan; Fischetti, Robert; Simpson, Garth J.

2013-01-01

Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ∼103–104-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering and analysis of phenylalanine hydroxylase from Chromobacterium violaceum cPAH, Trichinella spiralis deubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied. PMID:23765294

Three-dimensional distribution of polymorphs and magnesium in a calcified underwater attachment system by diffraction tomography

PubMed Central

Leemreize, Hanna; Almer, Jonathan D.; Stock, Stuart R.; Birkedal, Henrik

2013-01-01

Biological materials display complicated three-dimensional hierarchical structures. Determining these structures is essential in understanding the link between material design and properties. Herein, we show how diffraction tomography can be used to determine the relative placement of the calcium carbonate polymorphs calcite and aragonite in the highly mineralized holdfast system of the bivalve Anomia simplex. In addition to high fidelity and non-destructive mapping of polymorphs, we use detailed analysis of X-ray diffraction peak positions in reconstructed powder diffraction data to determine the local degree of Mg substitution in the calcite phase. These data show how diffraction tomography can provide detailed multi-length scale information on complex materials in general and of biomineralized tissues in particular. PMID:23804437

X-ray diffraction, spectroscopic and mechanical studies on potential organic NLO materials of metaNitroaniline and N-3-Nitrophenyl Acetamide single crystals

NASA Astrophysics Data System (ADS)

Senthil, S.; Madhavan, J.

2015-02-01

In the present paper, attempts were made to grow good quality metaNitroaniline (mNA) and N-3-Nitrophenyl (3-NAA) single crystals. The lattice parameter values from the Powder X-ray diffraction pattern confirms that mNA belongs to orthorhombic crystal system with the unit cell parameter values of a = 6.501 Å, b = 19.330 Å and c = 5.082 Å with space group Pbc21. Similarly the powder XRD data indicates that 3-NAA crystal retained its monoclinic structure with lattice parameter values a = 9.762 Å, b =13.287 Å, c =13.226 Å, and β = 102.99°. Investigation has been carried out to assign the vibrational frequencies of the grown crystals by Fourier Transform infrared spectroscopy technique. The SHG efficiency of mNA and 3NAA was determined by Kurtz and Perry powder technique. The Optical absorption study confirms the suitability of the crystals for device applications. The mechanical properties of the grown crystals have been studied using Vickers microhardness tester.

Compositional dependence of magnetic anisotropy in chemically synthesized Co3- x Fe x O4 (0 ≤ x ≤ 2)

NASA Astrophysics Data System (ADS)

Hayashi, Kensuke; Yamada, Keisuke; Shima, Mutsuhiro

2018-01-01

Magnetic anisotropy of Co3- x Fe x O4 (CFO, 0 ≤ x ≤ 2) thin-film and powder samples prepared by a sol-gel method has been investigated as a function of Fe composition x. Structural analyses by X-ray diffraction show that CFO powder samples exhibit diffraction peaks associated with the spinel structure when x < 2, while CFO thin-film samples with thickness of 130-510 nm yield the peaks when 0 ≤ x ≤ 2. CFO thin-film samples are highly (111)-oriented with the Lotgering factor greater than 0.9 when 0.6 ≤ x ≤ 1.3. The magnetic anisotropy constant K 1 of CFO powder samples estimated from their room-temperature hysteresis loops yields a minimum when x = 0.9. Relatively large in-plane magnetic anisotropy (K eff = 5.7 × 105 erg/cm3) is observed for the CFO thin-film sample when x = 1.3. With increasing x, the magnetic easy axis of the spinel CFO changes from 〈111〉 to 〈100〉 when x = 0.9.

An alternative gas sensor material: Synthesis and electrical characterization of SmCoO{sub 3}

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

Michel, Carlos Rafael; Delgado, Emilio; Santillan, Gloria

2007-01-18

Single-phase perovskite SmCoO{sub 3} was prepared by a wet-chemical synthesis technique using metal-nitrates and citric acid; after its characterization by thermal analyses and X-ray diffraction, sintering at 900 deg. C in air, gave single phase and well crystallized powders. The powders were mixed with an organic solvent to prepare a slurry, which was deposited on alumina substrates as thick films, using the screen-printing technique. Electrical and gas sensing properties of sintered SmCoO{sub 3} films were investigated in air, O{sub 2} and CO{sub 2}, the results show that sensitivity reached a maximum value at 420 deg. C, for both gases. Dynamicmore » tests revealed a better behavior of SmCoO{sub 3} in CO{sub 2} than O{sub 2}, due to a fast response and a larger electrical resistance change to this gas. X-ray diffraction made on powders after electrical characterization in gases, showed that perovskite-type structure was preserved.« less

Mechanically activated synthesis of PZT and its electromechanical properties

NASA Astrophysics Data System (ADS)

Liu, X.; Akdogan, E. K.; Safari, A.; Riman, R. E.

2005-08-01

Mechanical activation was successfully used to synthesize nanostructured phase-pure Pb(Zr0.7Ti0.3)O3 (PZT) powders. Lead zirconium titanium (PbZrTi) hydrous oxide precursor, synthesized from chemical co-precipitation, was mechanically activated in a NaCl matrix. The synthesized PZT particles were characterized by using X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, laser-light diffraction, and nitrogen adsorption. Thermogravimetric analysis and differential thermal analysis were used to monitor dehydration and phase transformation of PbZrTi hydrous oxide precursor during mechanical activation. The best mechanical activation conditions corresponded to mechanically activating PbZrTi hydrous oxide precursor in a NaCl matrix with a NaCl/precursor weight ratio of 4:1 for 8 h. These conditions resulted in a dispersible phase-pure PZT powder with a median secondary-particle size of ˜110 nm. The properties of PZT 70/30 from mechanically activated powder, as measured on discs sintered at 1150 °C for 2 h, were found to be in close conformity to those obtained by a conventional mixed oxide solid state reaction route.

Effect of Powder-Suspended Dielectric on the EDM Characteristics of Inconel 625

NASA Astrophysics Data System (ADS)

Talla, Gangadharudu; Gangopadhyay, S.; Biswas, C. K.

2016-02-01

The current work attempts to establish the criteria for powder material selection by investigating the influence of various powder-suspended dielectrics and machining parameters on various EDM characteristics of Inconel 625 (a nickel-based super alloy) which is nowadays regularly used in aerospace, chemical, and marine industries. The powders include aluminum (Al), graphite, and silicon (Si) that have significant variation in their thermo-physical characteristics. Results showed that powder properties like electrical conductivity, thermal conductivity, density, and hardness play a significant role in changing the machining performance and the quality of the machined surface. Among the three powders, highest material removal rate was observed for graphite powder due to its high electrical and thermal conductivities. Best surface finish and least radial overcut (ROC) were attained using Si powder. Maximum microhardness was found for Si due to its low thermal conductivity and high hardness. It is followed by graphite and aluminum powders. Addition of powder to the dielectric has increased the crater diameter due to expansion of plasma channel. Powder-mixed EDM (PMEDM) was also effective in lowering the density of surface cracks with least number of cracks obtained with graphite powder. X-ray diffraction analysis indicated possible formation of metal carbides along with grain growth phenomenon of Inconel 625 after PMEDM.

The Effect of Time, Temperature and Composition on Boron Carbide Synthesis by Sol-gel Method

NASA Astrophysics Data System (ADS)

Hadian, A. M.; Bigdeloo, J. A.

2008-02-01

To minimize free carbon residue in the boron carbide (B4C) powder, a modified sol-gel process is performed where the starting materials as boric acid and citric acid compositions are adjusted. Because of boron loss in the form of B2O2(g) during the reduction reaction of the stoichiometric starting composition, the final B4C powders contain carbon residues. Thus, an excess H3BO3 is used in the reaction to compensate the loss and to obtain stoichiometric powders. Parameters of production have been determined using x-ray diffraction analysis and particle size analyses. The synthesized B4C powder using an excess boric acid composition shows no trace of carbon.

Physicochemical characterization and water vapor sorption of organic solution advanced spray-dried inhalable trehalose microparticles and nanoparticles for targeted dry powder pulmonary inhalation delivery.

PubMed

Li, Xiaojian; Mansour, Heidi M

2011-12-01

Novel advanced spray-dried inhalable trehalose microparticulate/nanoparticulate powders with low water content were successfully produced by organic solution advanced spray drying from dilute solution under various spray-drying conditions. Laser diffraction was used to determine the volumetric particle size and size distribution. Particle morphology and surface morphology was imaged and examined by scanning electron microscopy. Hot-stage microscopy was used to visualize the presence/absence of birefringency before and following particle engineering design pharmaceutical processing, as well as phase transition behavior upon heating. Water content in the solid state was quantified by Karl Fisher (KF) coulometric titration. Solid-state phase transitions and degree of molecular order were examined by differential scanning calorimetry (DSC) and powder X-ray diffraction, respectively. Scanning electron microscopy showed a correlation between particle morphology, surface morphology, and spray drying pump rate. All advanced spray-dried microparticulate/nanoparticulate trehalose powders were in the respirable size range and exhibited a unimodal distribution. All spray-dried powders had very low water content, as quantified by KF. The absence of crystallinity in spray-dried particles was reflected in the powder X-ray diffractograms and confirmed by thermal analysis. DSC thermal analysis indicated that the novel advanced spray-dried inhalable trehalose microparticles and nanoparticles exhibited a clear glass transition (T(g)). This is consistent with the formation of the amorphous glassy state. Spray-dried amorphous glassy trehalose inhalable microparticles and nanoparticles exhibited vapor-induced (lyotropic) phase transitions with varying levels of relative humidity as measured by gravimetric vapor sorption at 25°C and 37°C.

Apparatus Notes.

ERIC Educational Resources Information Center

Eaton, Bruce G., Ed.

1982-01-01

Presents a technique to produce samples for x-ray diffraction studies on the Tel-X-Ometer 80 x-ray apparatus from readily available crystalline powders and discusses observations of transverse modes of an optical resonator. (SK)

Stepwise observation and quantification and mixed matrix membrane separation of CO2 within a hydroxy-decorated porous host† †Electronic supplementary information (ESI) available. CCDC 1504685–1504693. See DOI: 10.1039/c6sc04343g Click here for additional data file. Click here for additional data file.

PubMed Central

Morris, Christopher G.; Jacques, Nicholas M.; Godfrey, Harry G. W.; Mitra, Tamoghna; Fritsch, Detlev; Lu, Zhenzhong; Murray, Claire A.; Potter, Jonathan; Cobb, Tom M.; Yuan, Fajin

2017-01-01

The identification of preferred binding domains within a host structure provides important insights into the function of materials. State-of-the-art reports mostly focus on crystallographic studies of empty and single component guest-loaded host structures to determine the location of guests. However, measurements of material properties (e.g., adsorption and breakthrough of substrates) are usually performed for a wide range of pressure (guest coverage) and/or using multi-component gas mixtures. Here we report the development of a multifunctional gas dosing system for use in X-ray powder diffraction studies on Beamline I11 at Diamond Light Source. This facility is fully automated and enables in situ crystallographic studies of host structures under (i) unlimited target gas loadings and (ii) loading of multi-component gas mixtures. A proof-of-concept study was conducted on a hydroxyl-decorated porous material MFM-300(VIII) under (i) five different CO2 pressures covering the isotherm range and (ii) the loading of equimolar mixtures of CO2/N2. The study has successfully captured the structural dynamics underpinning CO2 uptake as a function of surface coverage. Moreover, MFM-300(VIII) was incorporated in a mixed matrix membrane (MMM) with PIM-1 in order to evaluate the CO2/N2 separation potential of this material. Gas permeation measurements on the MMM show a great improvement over the bare PIM-1 polymer for CO2/N2 separation based on the ideal selectivity. PMID:28507700

Crystallization of the photosystem II core complex and its chlorophyll binding subunit CP43 from transplastomic plants of Nicotiana tabacum.

PubMed

Piano, Dario; El Alaoui, Sabah; Korza, Henryk J; Filipek, Renata; Sabala, Izabela; Haniewicz, Patrycja; Buechel, Claudia; De Sanctis, Daniele; Bochtler, Matthias

2010-12-01

Photosystem II from transplastomic plants of Nicotiana tabacum with a hexahistidine tag at the N-terminal end of the PsbE subunit (α-chain of the cytochrome b(559)) was purified according to the protocol of Fey et al. (BBA 12:1501-1509, 2008). The protein sample was then subjected to two additional gel filtration runs in order to increase its homogeneity and to standardize the amount of detergent. Large three dimensional crystals of the core complex were obtained. Crystals of one of its chlorophyll binding subunits (CP43) in isolation grew in very similar conditions that differed only in the concentration of the detergent. Diffraction of Photosystem II and CP43 crystals at various synchrotron beamlines was limited to a resolution of 7 and 14 Å, respectively. In both cases the diffraction quality was insufficient for an unambiguous assignment of the crystallographic lattice or space group.

Crystallization of Δ1-tetrahydrocannabinolic acid (THCA) synthase from Cannabis sativa

PubMed Central

Shoyama, Yoshinari; Takeuchi, Ayako; Taura, Futoshi; Tamada, Taro; Adachi, Motoyasu; Kuroki, Ryota; Shoyama, Yukihiro; Morimoto, Satoshi

2005-01-01

Δ1-Tetrahydrocannabinolic acid (THCA) synthase is a novel oxidoreductase that catalyzes the biosynthesis of the psychoactive compound THCA in Cannabis sativa (Mexican strain). In order to investigate the structure–function relationship of THCA synthase, this enzyme was overproduced in insect cells, purified and finally crystallized in 0.1 M HEPES buffer pH 7.5 containing 1.4 M sodium citrate. A single crystal suitable for X-ray diffraction measurement was obtained in 0.09 M HEPES buffer pH 7.5 containing 1.26 M sodium citrate. The crystal diffracted to 2.7 Å resolution at beamline BL41XU, SPring-8. The crystal belonged to the primitive cubic space group P432, with unit-cell parameters a = b = c = 178.2 Å. The calculated Matthews coefficient was approximately 4.1 or 2.0 Å3 Da−1 assuming the presence of one or two molecules of THCA synthase in the asymmetric unit, respectively. PMID:16511162

New Python-based methods for data processing

PubMed Central

Sauter, Nicholas K.; Hattne, Johan; Grosse-Kunstleve, Ralf W.; Echols, Nathaniel

2013-01-01

Current pixel-array detectors produce diffraction images at extreme data rates (of up to 2 TB h−1) that make severe demands on computational resources. New multiprocessing frameworks are required to achieve rapid data analysis, as it is important to be able to inspect the data quickly in order to guide the experiment in real time. By utilizing readily available web-serving tools that interact with the Python scripting language, it was possible to implement a high-throughput Bragg-spot analyzer (cctbx.spotfinder) that is presently in use at numerous synchrotron-radiation beamlines. Similarly, Python interoperability enabled the production of a new data-reduction package (cctbx.xfel) for serial femto­second crystallography experiments at the Linac Coherent Light Source (LCLS). Future data-reduction efforts will need to focus on specialized problems such as the treatment of diffraction spots on interleaved lattices arising from multi-crystal specimens. In these challenging cases, accurate modeling of close-lying Bragg spots could benefit from the high-performance computing capabilities of graphics-processing units. PMID:23793153

Diffracting aperture based differential phase contrast for scanning X-ray microscopy.

PubMed

Kaulich, Burkhard; Polack, Francois; Neuhaeusler, Ulrich; Susini, Jean; di Fabrizio, Enzo; Wilhein, Thomas

2002-10-07

It is demonstrated that in a zone plate based scanning X-ray microscope, used to image low absorbing, heterogeneous matter at a mesoscopic scale, differential phase contrast (DPC) can be implemented without adding any additional optical component to the normal scheme of the microscope. The DPC mode is simply generated by an appropriate positioning and alignment of microscope apertures. Diffraction from the apertures produces a wave front with a non-uniform intensity. The signal recorded by a pinhole photo diode located in the intensity gradient is highly sensitive to phase changes introduced by the specimen to be recorded. The feasibility of this novel DPC technique was proven with the scanning X-ray microscope at the ID21 beamline of the European Synchrotron Radiation facility (ESRF) operated at 6 keV photon energy. We observe a differential phase contrast, similar to Nomarski's differential interference contrast for the light microscope, which results in a tremendous increase in image contrast of up to 20 % when imaging low absorbing specimen.

Optics for coherent X-ray applications.

PubMed

Yabashi, Makina; Tono, Kensuke; Mimura, Hidekazu; Matsuyama, Satoshi; Yamauchi, Kazuto; Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

2014-09-01

Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed.

Broadband X-ray edge-enhancement imaging of a boron fibre on lithium fluoride thin film detector

NASA Astrophysics Data System (ADS)

Nichelatti, E.; Bonfigli, F.; Vincenti, M. A.; Cecilia, A.; Vagovič, P.; Baumbach, T.; Montereali, R. M.

2016-10-01

The white beam (∼6-80 keV) available at the TopoTomo X-ray beamline of the ANKA synchrotron facility (KIT, Karlsruhe, Germany) was used to perform edge-enhancement imaging tests on lithium fluoride radiation detectors. The diffracted X-ray image of a microscopic boron fibre, consisting of tungsten wire wrapped by boron cladding, was projected onto lithium fluoride thin films placed at several distances, from contact to 1 m . X-ray photons cause the local formation of primary and aggregate colour centres in lithium fluoride; these latter, once illuminated under blue light, luminesce forming visible-light patterns-acquired by a confocal laser scanning microscope-that reproduce the intensity of the X-ray diffracted images. The tests demonstrated the excellent performances of lithium fluoride films as radiation detectors at the investigated photon energies. The experimental results are here discussed and compared with those calculated with a model that takes into account all the processes that concern image formation, storing and readout.

Structure determination of an integral membrane protein at room temperature from crystals in situ

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

Axford, Danny; Foadi, James; Imperial College London, London SW7 2AZ

2015-05-14

The X-ray structure determination of an integral membrane protein using synchrotron diffraction data measured in situ at room temperature is demonstrated. The structure determination of an integral membrane protein using synchrotron X-ray diffraction data collected at room temperature directly in vapour-diffusion crystallization plates (in situ) is demonstrated. Exposing the crystals in situ eliminates manual sample handling and, since it is performed at room temperature, removes the complication of cryoprotection and potential structural anomalies induced by sample cryocooling. Essential to the method is the ability to limit radiation damage by recording a small amount of data per sample from many samplesmore » and subsequently assembling the resulting data sets using specialized software. The validity of this procedure is established by the structure determination of Haemophilus influenza TehA at 2.3 Å resolution. The method presented offers an effective protocol for the fast and efficient determination of membrane-protein structures at room temperature using third-generation synchrotron beamlines.« less

Crystallization and preliminary X-ray crystallographic analysis of the GluR0 ligand-binding core from Nostoc punctiforme

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

Lee, Jun Hyuck; Park, Soo Jeong; Rho, Seong-Hwan

2005-11-01

The GluR0 ligand-binding core from N. punctiforme was expressed, purified and crystallized in the presence of l-glutamate. A diffraction data set was collected to a resolution of 2.1 Å. GluR0 from Nostoc punctiforme (NpGluR0) is a bacterial homologue of the ionotropic glutamate receptor. The ligand-binding core of NpGluR0 was crystallized at 294 K using the hanging-drop vapour-diffusion method. The l-glutamate-complexed crystal belongs to space group C222{sub 1}, with unit-cell parameters a = 78.0, b = 145.1, c = 132.1 Å. The crystals contain three subunits in the asymmetric unit, with a V{sub M} value of 2.49 Å{sup 3} Da{sup −1}.more » The diffraction limit of the l-glutamate complex data set was 2.1 Å using synchrotron X-ray radiation at beamline BL-4A of the Pohang Accelerator Laboratory (Pohang, Korea)« less