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Sample records for single crystal diffraction

  1. Diffraction. Single crystal, magnetic

    International Nuclear Information System (INIS)

    Heger, G.

    1999-01-01

    The analysis of crystal structure and magnetic ordering is usually based on diffraction phenomena caused by the interaction of matter with X-rays, neutrons, or electrons. Complementary information is achieved due to the different character of X-rays, neutrons and electrons, and hence their different interactions with matter and further practical aspects. X-ray diffraction using conventional laboratory equipment and/or synchrotron installations is the most important method for structure analyses. The purpose of this paper is to discuss special cases, for which, in addition to this indispensable part, neutrons are required to solve structural problems. Even though the huge intensity of modern synchrotron sources allows in principle the study of magnetic X-ray scattering the investigation of magnetic structures is still one of the most important applications of neutron diffraction. (K.A.)

  2. Neutron forward diffraction by single crystal prisms

    Indian Academy of Sciences (India)

    We have derived analytic expressions for the deflection as well as transmitted fraction of monochromatic neutrons forward diffracted by a single crystal prism. In the vicinity of a Bragg reflection, the neutron deflection deviates sharply from that for an amorphous prism, exhibiting three orders of magnitude greater sensitivity to ...

  3. Trapezoidal diffraction grating beam splitters in single crystal diamond

    Science.gov (United States)

    Kiss, Marcell; Graziosi, Teodoro; Quack, Niels

    2018-02-01

    Single Crystal Diamond has been recognized as a prime material for optical components in high power applications due to low absorption and high thermal conductivity. However, diamond microstructuring remains challenging. Here, we report on the fabrication and characterization of optical diffraction gratings exhibiting a symmetric trapezoidal profile etched into a single crystal diamond substrate. The optimized grating geometry diffracts the transmitted optical power into precisely defined proportions, performing as an effective beam splitter. We fabricate our gratings in commercially available single crystal CVD diamond plates (2.6mm x 2.6mm x 0.3mm). Using a sputter deposited hard mask and patterning by contact lithography, the diamond is etched in an inductively coupled oxygen plasma with zero platen power. The etch process effectively reveals the characteristic {111} diamond crystal planes, creating a precisely defined angled (54.7°) profile. SEM and AFM measurements of the fabricated gratings evidence the trapezoidal shape with a pitch of 3.82μm, depth of 170 nm and duty cycle of 35.5%. Optical characterization is performed in transmission using a 650nm laser source perpendicular to the sample. The recorded transmitted optical power as function of detector rotation angle shows a distribution of 21.1% in the 0th order and 23.6% in each +/-1st order (16.1% reflected, 16.6% in higher orders). To our knowledge, this is the first demonstration of diffraction gratings with trapezoidal profile in single crystal diamond. The fabrication process will enable beam splitter gratings of custom defined optical power distribution profiles, while antireflection coatings can increase the efficiency.

  4. The CCP14 for single crystal and powder diffraction

    International Nuclear Information System (INIS)

    Cranswick, L.M.D.

    1999-01-01

    Full text: The Collaborative Computation Project Number 14 for Single Crystal and Powder Diffraction (CCP14) is continuing in its objective to provide freely available software and resources for the powder diffraction and crystallographic community. Using the Internet and World Wide Web, we are presently compiling software and web resources, creating tutorials and help files. It also endeavours to encourage and provide resources to assist program authors with developing their software. The CCP14 presently has its web-site at and a mirror at (at CSIRO, Melbourne, Australia). Auto web-mirroring is being implemented to allow users to obtain software and access to resources in a more time effective manner. For people in countries isolated from the Internet, the CCP14 on CD-ROM can be snail mailed on request. This is in the form of a Virtual World Wide Web/Virtual Internet; in the same vein as the existing Crystallographic Nexus CD-ROM. Copyright (1999) Australian X-ray Analytical Association Inc

  5. Photoelectron diffraction studies of small adsorbates on single crystal surfaces

    International Nuclear Information System (INIS)

    Pascal, Mathieu

    2002-01-01

    The structural determination of small molecules adsorbed on single crystal surfaces has been investigated using scanned energy mode photoelectron diffraction (PhD). The experimental PhD data were compared to theoretical models using a simulation program based on multiple scattering calculations. Three adsorption systems have been examined on Ag(110), Cu(110) and Cu(111) crystals. The structure of the (2x1)-O adsorption phase on Ag(110) revealed that the O atoms occupied the long bridge site and are almost co-planar with the top layer of Ag atoms. The best agreement between multiple scattering theory and experiment has been obtained for a missing-row (or equivalently an 'added- row') reconstruction. Alternative buckled-row and unreconstructed surface models can be excluded. The adsorption of the benzoate species on Cu(110) has been found to occur via the carboxylate group. The molecules occupy short bridge sites with the O atoms being slightly displaced from atop sites and are aligned along the close-packed azimuth. The tilt of the molecule with respect to the surface and the degree to which the surface is relaxed have also been investigated. The adsorption of methyl on Cu(111) was studied using either azomethane or methyl iodide to prepare the surface layers. At saturation coverage the preferred adsorption site is the fcc threefold hollow site, whereas at half saturation coverage ∼ 30 % of the methyl species occupy the hop threefold hollow sites. Best agreement between theory and experiment corresponded to a methyl group adsorbed with C 3v symmetry. The height of the C above the surface in a pure methyl layer was 1.66 ± 0.02 A, but was reduced to 1.62 ± 0.02 A in the presence of co-adsorbed iodine, suggesting that iodine increases the strength of adsorption. Iodine was also found to occupy the fee threefold hollow sites with a Cu-l bondlength of 2.61 ± 0.02 A. (author)

  6. Diffraction and single-crystal elastic constants of Inconel 625 at room and elevated temperatures determined by neutron diffraction

    International Nuclear Information System (INIS)

    Wang, Zhuqing; Stoica, Alexandru D.; Ma, Dong; Beese, Allison M.

    2016-01-01

    In this work, diffraction and single-crystal elastic constants of Inconel 625 have been determined by means of in situ loading at room and elevated temperatures using time-of-flight neutron diffraction. Theoretical models proposed by Voigt, Reuss, and Kroner were used to determine single-crystal elastic constants from measured diffraction elastic constants, with the Kroner model having the best ability to capture experimental data. The magnitude of single-crystal elastic moduli, computed from single-crystal elastic constants, decreases and the single crystal anisotropy increases as temperature increases, indicating the importance of texture in affecting macroscopic stress at elevated temperatures. The experimental data reported here are of great importance in understanding additive manufacturing of metallic components as: diffraction elastic constants are required for computing residual stresses from residual lattice strains measured using neutron diffraction, which can be used to validate thermomechanical models of additive manufacturing, while single-crystal elastic constants can be used in crystal plasticity modeling, for example, to understand mechanical deformation behavior of additively manufactured components.

  7. Diffraction and single-crystal elastic constants of Inconel 625 at room and elevated temperatures determined by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Zhuqing [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States); Stoica, Alexandru D. [Chemical and Engineering Materials Division, Neutron Sciences Directorate, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Ma, Dong, E-mail: dongma@ornl.gov [Chemical and Engineering Materials Division, Neutron Sciences Directorate, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Beese, Allison M., E-mail: amb961@psu.edu [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States)

    2016-09-30

    In this work, diffraction and single-crystal elastic constants of Inconel 625 have been determined by means of in situ loading at room and elevated temperatures using time-of-flight neutron diffraction. Theoretical models proposed by Voigt, Reuss, and Kroner were used to determine single-crystal elastic constants from measured diffraction elastic constants, with the Kroner model having the best ability to capture experimental data. The magnitude of single-crystal elastic moduli, computed from single-crystal elastic constants, decreases and the single crystal anisotropy increases as temperature increases, indicating the importance of texture in affecting macroscopic stress at elevated temperatures. The experimental data reported here are of great importance in understanding additive manufacturing of metallic components as: diffraction elastic constants are required for computing residual stresses from residual lattice strains measured using neutron diffraction, which can be used to validate thermomechanical models of additive manufacturing, while single-crystal elastic constants can be used in crystal plasticity modeling, for example, to understand mechanical deformation behavior of additively manufactured components.

  8. Single-crystal diffraction instrument TriCS at SINQ

    Science.gov (United States)

    Schefer, J.; Könnecke, M.; Murasik, A.; Czopnik, A.; Strässle, Th; Keller, P.; Schlumpf, N.

    2000-03-01

    The single-crystal diffractometer TriCS at the Swiss Continuous Spallation Source (SINQ) is presently in the commissioning phase. A two-dimensional wire detector produced by EMBL was delivered in March 1999. The instrument is presently tested with a single detector. First measurements on magnetic structures have been performed. The instrument is remotely controlled using JAVA-based software and a UNIX DEC-α host computer.

  9. Corelli: Efficient single crystal diffraction with elastic discrimination

    Indian Academy of Sciences (India)

    Here, we discuss the potential of the cross-correlation technique for efficient measurement of single crystal diffuse scattering with energy discrimination, as will be implemented in a novel instrument, Corelli. Utilizing full experiment simulations, we show that this technique readily leads up to a fifty-fold gain in efficiency, ...

  10. Twinning processes in Cu-Al-Ni martensite single crystals investigated by neutron single crystal diffraction method

    Czech Academy of Sciences Publication Activity Database

    Molnar, P.; Šittner, P.; Novák, V.; Lukáš, Petr

    2008-01-01

    Roč. 481, Sp.Iss.SI (2008), s. 513-517 ISSN 0921-5093 R&D Projects: GA AV ČR IAA100480704 Institutional research plan: CEZ:AV0Z10480505 Keywords : Cu-Al-Ni * single crystals * neutron diffraction Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 1.806, year: 2008

  11. Twinning processes in Cu-Al-Ni martensite single crystals investigated by neutron single crystal diffraction method

    International Nuclear Information System (INIS)

    Molnar, P.; Sittner, P.; Novak, V.; Lukas, P.

    2008-01-01

    A neutron single crystal diffraction method for inspecting the quality of martensite single crystals is introduced. True interface-free martensite single crystals are indispensable for, e.g. measurement of elastic constants of phases by ultrasonic techniques. The neutron diffraction method was used to detect and distinguish the presence of individual lattice correspondence variants of the 2H orthorhombic martensite phase in Cu-Al-Ni as well as to follow the activity of twinning processes during the deformation test on the martensite variant single crystals. When preparing the martensite single variant prism-shaped crystals by compression deformation method, typically a small fraction of second unwanted martensitic variant (compound twin) remains in the prism samples. Due to the very low stress (∼1 MPa) for the compound twinning in many shape memory alloys, it is quite difficult not only to deplete the martensite prisms of all internal interfaces but mainly to keep them in the martensite single variant state for a long time needed for further investigations

  12. Advanced x-ray stress analysis method for a single crystal using different diffraction plane families

    International Nuclear Information System (INIS)

    Imafuku, Muneyuki; Suzuki, Hiroshi; Sueyoshi, Kazuyuki; Akita, Koichi; Ohya, Shin-ichi

    2008-01-01

    Generalized formula of the x-ray stress analysis for a single crystal with unknown stress-free lattice parameter was proposed. This method enables us to evaluate the plane stress states with any combination of diffraction planes. We can choose and combine the appropriate x-ray sources and diffraction plane families, depending on the sample orientation and the apparatus, whenever diffraction condition is satisfied. The analysis of plane stress distributions in an iron single crystal was demonstrated combining with the diffraction data for Fe{211} and Fe{310} plane families

  13. Anomalous effect of high-frequency ultrasound on radiation diffraction in deformed single crystals

    International Nuclear Information System (INIS)

    Iolin, E.M.; Rajtman, Eh.A.; Kuvaldin, B.V.; Zolotoyabko, Eh.V.

    1988-01-01

    Results are presented of a theoretical and experimental study of neutron and X-ray diffraction in defromed single crystals on high-frequency ultrasonic excitation. It is demonstrated theoretically that at a frequency exceeding a certain threshold value the ultrasound violates the adiabatic conditions for the excitation point motion on the dispersion surface branches. This leads to an anomalous (compared to diffraction for a perfect crystal) dependence of the diffraction intensity on the ultrasonic wave amplitude. The experimental data for Si crystals are in good agreement with the theoretical predictions

  14. Single-Crystal Diffraction from Two-Dimensional Block Copolymer Arrays

    International Nuclear Information System (INIS)

    Stein, G. E.; Kramer, E. J.; Li, X.; Wang, J.

    2007-01-01

    The structure of oriented 2D block copolymer single crystals is characterized by grazing-incidence small-angle x-ray diffraction, demonstrating long-range sixfold orientational order. From line shape analysis of the higher-order Bragg diffraction peaks, we determine that translational order decays algebraically with a decay exponent η=0.2, consistent with the Kosterlitz-Thouless-Halperin-Nelson-Young theory for a 2D crystal with a shear modulus μ=2x10 -4 N/m

  15. Thermal diffuse scattering in time-of-flight neutron diffraction studied on SBN single crystals

    International Nuclear Information System (INIS)

    Prokert, F.; Savenko, B.N.; Balagurov, A.M.

    1994-01-01

    At time-of-flight (TOF) diffractometer D N-2, installed at the pulsed reactor IBR-2 in Dubna, Sr x Ba 1-x Nb 2 O 6 mixed single crystals (SBN-x) of different compositions (0.50 < x< 0.75) were investigated between 15 and 773 K. The diffraction patterns were found to be strongly influenced by the thermal diffuse scattering (TDS). The appearance of the TDS from the long wavelength acoustic models of vibration in single crystals is characterized by the ratio of the velocity of sound to the velocity of neutron. Due to the nature of the TOF Laue diffraction technique used on D N-2, the TDS around Bragg peaks has rather a complex profile. An understanding of the TDS close to Bragg peaks is essential in allowing the extraction of the diffuse scattering occurring at the diffuse ferroelectric phase transition in SBN crystals. 11 refs.; 9 figs.; 1 tab. (author)

  16. About some practical aspects of X-ray diffraction : From single crystal to powders

    Energy Technology Data Exchange (ETDEWEB)

    Giacovazzo, C [Bari Univ. (Italy). Dip. Geomineralogico

    1996-09-01

    An ideal polycrystalline material or power is an ensemble of a very large number of randomly oriented crystallites. It is shown the effect that this random orientation has on the diffraction of a specimen assumed to contain only one reciprocal lattice node. The most remarkable difference with the single-crystal case is that now must think of scattering vectors not as lying on discrete nodes of reciprocal lattice vectors, the distances from the single-crystal reciprocal lattice nodes to the origin of reciprocal space.

  17. About some practical aspects of X-ray diffraction : From single crystal to powders

    International Nuclear Information System (INIS)

    Giacovazzo, C.

    1996-01-01

    An ideal polycrystalline material or power is an ensemble of a very large number of randomly oriented crystallites. It is shown the effect that this random orientation has on the diffraction of a specimen assumed to contain only one reciprocal lattice node. The most remarkable difference with the single-crystal case is that now must think of scattering vectors not as lying on discrete nodes of reciprocal lattice vectors, the distances from the single-crystal reciprocal lattice nodes to the origin of reciprocal space

  18. Single-crystal neutron diffraction study of ammonium nitrate phase III

    International Nuclear Information System (INIS)

    Choi, C.S.; Prask, H.J.

    1982-01-01

    The crystal structure of ammonium nitrate phase III has been studied at room temperature by neutron diffraction using a single crystal containing 5% KNO 3 in solid-solution form. The space group is Pnma, with a = 7.6772 (4), b = 5.8208 (4), c = 7.1396 (5) A, Z = 4. The final residual after full-matrix least-squares refinement was R = 0.042 for 348 observed reflections. The ammonium ions are thermally disordered into two orientations, displaced by an angle of approximately 42 0 about an axis parallel to the c axis. (Auth.)

  19. Single-crystal neutron diffraction at the Australian Replacement Research Reactor

    International Nuclear Information System (INIS)

    Klooster, W.T.

    2001-01-01

    The purpose of the workshop was to: identify the future needs and opportunities for single-crystal neutron diffraction, and specify instrument requirements. important number of experiments. The conclusion of the workshop deliberation was that Australia has a diverse community of users of single-crystal neutron diffraction. A (quasi)-Laue image-plate diffractometer allows the fastest throughput by far, but would exclude an important number of experiments. Most of these could be covered by the additional possibility to locate the image-plate detector on a monochromatic beam. Therefore it was recommend both a white thermal beam and a monochromatic beam (λ= 1 to 2.4 Angstroms) for an image-plate detector. At little additional cost the existing 2TanA instrument could be located semi-permanently on the same monochromatic beam, thus offering three quite different types of single-crystal instruments. Small improvements could be made to the 2TanA instrument to cater for the remaining experiments not suited to an image-plate diffractometer: exchange of the Eulerian cradle for an automated tilt goniometer for extremely bulky sample environment (cryomagnets, large pressure cells), optional larger area detector, analyser crystal. It was recommended that an Instrument Advisory Team will be assembled, and will help in specifying, designing and commissioning the instrument

  20. Single-crystal neutron diffraction studies of hydrogen-bonded systems: Two recent examples from IPNS

    Energy Technology Data Exchange (ETDEWEB)

    Koetzle, Thomas F. [IPNS Division, Argonne National Laboratory, Argonne, IL 60439 (United States)], E-mail: tkoetzle@anl.gov; Piccoli, Paula M.B.; Schultz, Arthur J. [IPNS Division, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2009-02-21

    Beginning with work in the 1950s at the first generation of research reactors, studies of hydrogen-bonded systems have been a prime application for single-crystal neutron diffraction. The range of systems studied was extended in the 1960s and 1970s, with the advent of high flux reactor sources, and beginning around 1980 studies at pulsed neutron sources have made increasingly important contributions. Recently at the Argonne Intense Pulsed Neutron Source (IPNS), working with collaborators, we completed two studies of hydrogen-bonded systems that will serve to illustrate topics of current interest. In the first study, on andrographolide, an active diterpenoid natural product, our neutron diffraction results definitively characterize the hydrogen-bonding interactions. The second IPNS study is on tetraacetylethane (TAE), a {beta}-diketone enol system with a very short, strong intramolecular O-H...O hydrogen bond. At IPNS, we have determined the neutron crystal structure of TAE at five temperatures between 20 and 298 K to investigate changes in the structure with temperature and to probe for disorder. Despite the successes illustrated by the two examples presented here and by many other studies, at present applications of single-crystal neutron diffraction continue to be extremely flux limited and constrained by the requirement for mm-size crystals for many problems. These limitations are being addressed through the realization of powerful instruments at a new generation of pulsed neutron sources, including in the USA the TOPAZ and MaNDi single-crystal diffractometers that are under development at the Spallation Neutron Source (SNS)

  1. Single-crystal neutron diffraction studies of hydrogen-bonded systems: Two recent examples from IPNS

    Science.gov (United States)

    Koetzle, Thomas F.; Piccoli, Paula M. B.; Schultz, Arthur J.

    2009-02-01

    Beginning with work in the 1950s at the first generation of research reactors, studies of hydrogen-bonded systems have been a prime application for single-crystal neutron diffraction. The range of systems studied was extended in the 1960s and 1970s, with the advent of high flux reactor sources, and beginning around 1980 studies at pulsed neutron sources have made increasingly important contributions. Recently at the Argonne Intense Pulsed Neutron Source (IPNS), working with collaborators, we completed two studies of hydrogen-bonded systems that will serve to illustrate topics of current interest. In the first study, on andrographolide, an active diterpenoid natural product, our neutron diffraction results definitively characterize the hydrogen-bonding interactions. The second IPNS study is on tetraacetylethane (TAE), a β-diketone enol system with a very short, strong intramolecular O-H⋯O hydrogen bond. At IPNS, we have determined the neutron crystal structure of TAE at five temperatures between 20 and 298 K to investigate changes in the structure with temperature and to probe for disorder. Despite the successes illustrated by the two examples presented here and by many other studies, at present applications of single-crystal neutron diffraction continue to be extremely flux limited and constrained by the requirement for mm-size crystals for many problems. These limitations are being addressed through the realization of powerful instruments at a new generation of pulsed neutron sources, including in the USA the TOPAZ and MaNDi single-crystal diffractometers that are under development at the Spallation Neutron Source (SNS).

  2. Single-crystal neutron diffraction studies of hydrogen-bonded systems: Two recent examples from IPNS

    International Nuclear Information System (INIS)

    Koetzle, Thomas F.; Piccoli, Paula M.B.; Schultz, Arthur J.

    2009-01-01

    Beginning with work in the 1950s at the first generation of research reactors, studies of hydrogen-bonded systems have been a prime application for single-crystal neutron diffraction. The range of systems studied was extended in the 1960s and 1970s, with the advent of high flux reactor sources, and beginning around 1980 studies at pulsed neutron sources have made increasingly important contributions. Recently at the Argonne Intense Pulsed Neutron Source (IPNS), working with collaborators, we completed two studies of hydrogen-bonded systems that will serve to illustrate topics of current interest. In the first study, on andrographolide, an active diterpenoid natural product, our neutron diffraction results definitively characterize the hydrogen-bonding interactions. The second IPNS study is on tetraacetylethane (TAE), a β-diketone enol system with a very short, strong intramolecular O-H...O hydrogen bond. At IPNS, we have determined the neutron crystal structure of TAE at five temperatures between 20 and 298 K to investigate changes in the structure with temperature and to probe for disorder. Despite the successes illustrated by the two examples presented here and by many other studies, at present applications of single-crystal neutron diffraction continue to be extremely flux limited and constrained by the requirement for mm-size crystals for many problems. These limitations are being addressed through the realization of powerful instruments at a new generation of pulsed neutron sources, including in the USA the TOPAZ and MaNDi single-crystal diffractometers that are under development at the Spallation Neutron Source (SNS).

  3. I19, the small-molecule single-crystal diffraction beamline at Diamond Light Source.

    Science.gov (United States)

    Nowell, Harriott; Barnett, Sarah A; Christensen, Kirsten E; Teat, Simon J; Allan, David R

    2012-05-01

    The dedicated small-molecule single-crystal X-ray diffraction beamline (I19) at Diamond Light Source has been operational and supporting users for over three years. I19 is a high-flux tunable-wavelength beamline and its key details are described in this article. Much of the work performed on the beamline involves structure determination from small and weakly diffracting crystals. Other experiments that have been supported to date include structural studies at high pressure, studies of metastable species, variable-temperature crystallography, studies involving gas exchange in porous materials and structural characterizations that require analysis of the diffuse scattering between Bragg reflections. A range of sample environments to facilitate crystallographic studies under non-ambient conditions are available as well as a number of options for automation. An indication of the scope of the science carried out on the beamline is provided by the range of highlights selected for this paper.

  4. Phase transition sequence in ferroelectric Aurivillius compounds investigated by single crystal X-ray diffraction

    Science.gov (United States)

    Boullay, P.; Tellier, J.; Mercurio, D.; Manier, M.; Zuñiga, F. J.; Perez-Mato, J. M.

    2012-09-01

    The investigation of the phase transition sequence in SrBi2Ta2O9 (SBT) and SrBi2Nb2O9 (SBN) is reported using single-crystal X-ray diffraction. By monitoring specific reflections as a function of temperature, sensitive either to the superstructure formation or to polar displacements, it was possible to check the existence or not of an intermediate phase. This latter was confirmed in SBT, but within experimental accuracy could not be detected in SBN.

  5. Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

    Science.gov (United States)

    Lunt, A. J. G.; Xie, M. Y.; Baimpas, N.; Zhang, S. Y.; Kabra, S.; Kelleher, J.; Neo, T. K.; Korsunsky, A. M.

    2014-08-01

    Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals. Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.

  6. Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

    Energy Technology Data Exchange (ETDEWEB)

    Lunt, A. J. G., E-mail: alexander.lunt@eng.ox.ac.uk; Xie, M. Y.; Baimpas, N.; Korsunsky, A. M. [Department of Engineering Science, University of Oxford, Parks Road, Oxford OX1 3PJ (United Kingdom); Zhang, S. Y.; Kabra, S.; Kelleher, J. [ISIS Neutron and Muon Source, Rutherford Appleton Laboratory, Harwell, Oxford OX11 0QX (United Kingdom); Neo, T. K. [Specialist Dental Group, Mount Elizabeth Orchard, 3 Mount Elizabeth, #08-03/08-08/08-10, Singapore 228510 (Singapore)

    2014-08-07

    Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals. Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.

  7. 40-Tesla pulsed-field cryomagnet for single crystal neutron diffraction

    Science.gov (United States)

    Duc, F.; Tonon, X.; Billette, J.; Rollet, B.; Knafo, W.; Bourdarot, F.; Béard, J.; Mantegazza, F.; Longuet, B.; Lorenzo, J. E.; Lelièvre-Berna, E.; Frings, P.; Regnault, L.-P.

    2018-05-01

    We present the first long-duration and high duty cycle 40-T pulsed-field cryomagnet addressed to single crystal neutron diffraction experiments at temperatures down to 2 K. The magnet produces a horizontal field in a bi-conical geometry, ±15° and ±30° upstream and downstream of the sample, respectively. Using a 1.15 MJ mobile generator, magnetic field pulses of 100 ms length are generated in the magnet, with a rise time of 23 ms and a repetition rate of 6-7 pulses per hour at 40 T. The setup was validated for neutron diffraction on the CEA-CRG three-axis spectrometer IN22 at the Institut Laue Langevin.

  8. X-ray diffraction patterns of single crystals implanted with high-energy light ions

    International Nuclear Information System (INIS)

    Wieteska, K.

    1998-01-01

    X-ray diffraction patterns of silicon and gallium arsenide single crystals implanted with high-energy protons and α-particles were studied. A various models of lattice parameter changes were analysed. The agreement between the simulation and experiment proves that the lattice parameter depth-distribution can be assumed to be proportional to vacancy distribution obtained by Monte-Carlo method and from the Biersack-Ziegler theory. Most of the X-ray experiments were performed using synchrotron source of X-ray radiation in particular in the case of back-reflection and transmission section topographic methods. The new method of direct determination of the implanted ion ranges was proposed using synchrotron radiation back-reflection section topography. A number of new interference phenomena was revealed and explained. These interferences are important in the applications of diffraction theory in studying of the real structure of implanted layers. (author)

  9. A diamond-anvil high-pressure cell for X-ray diffraction on a single crystal

    International Nuclear Information System (INIS)

    Malinowski, M.

    1987-01-01

    A new diamond-anvil high-pressure cell is described which can be used in single-crystal X-ray diffraction instruments to collect X-ray intensity data from single-crystal samples up to hydrostatic pressures of about 10 GPa. A unique design allows two types of diffraction geometry to be applied in single-crystal high-pressure diffraction experiments. More than 85% of the Ewald sphere is accessible, and a continuous range of 2θ values is available from 0 up to about 160 0 . Pressure may be calibrated by the ruby fluorescence technique or by the use of an internal X-ray-standard single crystal. The design of our diamond-anvil cell would allow, with little or no modification, operation at high and low temperatures, optical studies and powder diffractometer work. (orig.)

  10. X-ray diffraction studies of NbTe 2 single crystal

    Indian Academy of Sciences (India)

    The composition of the grown crystals was confirmed on the basis of energy dispersive analysis by X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and X-ray density have been carried out for the grown crystals. The particle size ...

  11. Simultaneous X-ray diffraction from multiple single crystals of macromolecules

    DEFF Research Database (Denmark)

    Paithankar, Karthik S.; Sørensen, Henning Osholm; Wright, Jonathan P.

    2011-01-01

    The potential in macromolecular crystallography for using multiple crystals to collect X-ray diffraction data simultaneously from assemblies of up to seven crystals is explored. The basic features of the algorithms used to extract data and their practical implementation are described. The procedure...

  12. Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

    Science.gov (United States)

    Tang, M X; Zhang, Y Y; E, J C; Luo, S N

    2018-05-01

    Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

  13. Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

    Energy Technology Data Exchange (ETDEWEB)

    Tang, M. X.; Zhang, Y. Y.; E, J. C.; Luo, S. N.

    2018-04-24

    Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

  14. Investigation of the neutron diffraction anomaly and electrical behaviour of α-LiIO3 single crystal under AC field

    International Nuclear Information System (INIS)

    Wang Guang; Yang Zhen

    1990-01-01

    A systematic study of the unique neutron diffraction and electric behaviour of α-LiIO 3 single crystal under AC field is reported. A frequency dependent rectification effect was observed and can be explained as the relaxation process in the ionic conduction. Theoretical treatment using Boltzmann equation gives satisfactory agreement with experimental results. The neutron diffraction anomaly can be attributed to the effect of the rectified DC current in the sample

  15. Stress-induced martensite variant reorientation in magnetic shape memory Ni–Mn–Ga single crystal studied by neutron diffraction

    Czech Academy of Sciences Publication Activity Database

    Molnár, Peter; Šittner, Petr; Lukáš, Petr; Hannula, S.-P.; Heczko, Oleg

    2008-01-01

    Roč. 17, č. 3 (2008), 035014/1-035014/4 ISSN 0964-1726 Institutional research plan: CEZ:AV0Z10100520; CEZ:AV0Z10480505 Keywords : NiMnGa single crystal * neutron diffraction * stress induced martensite reorientation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.743, year: 2008

  16. Single crystal neutron diffraction study of SrFeOsub(3-x)(x=0. 1)

    Energy Technology Data Exchange (ETDEWEB)

    Oda, H; Yamaguchi, Y; Takei, H; Watanabe, H [Tohoku Univ., Sendai (Japan). Research Inst. for Iron, Steel and Other Metals

    1977-01-01

    Neutron diffraction study was carried out on single crystals of the perovskite oxide SrFeOsub(3-x)(x=0.1). SrFeOsub(3-x)(x=0.1) has a proper screw spin structure with the propagation vector parallel to (111) direction and its Neel temperature is 118 K. The electron configuration of Fe/sup 4 +/(3d/sup 4/) ion is close to the low-spin state (tsub(2g)sup(4)) and the oxygen ion has the unpaired electron with the magnetic moment of 0.3..mu..sub(B) antiparallel to the vector sum of the magnetic moments of two iron ions lying on the neighbouring planes perpendicular to the screw axis. The absolute value of the propagation vector is almost constant. 0.130x..sqrt..3.2..pi../a A/sup -1/, at temperatures below 50 K, while it decreases gradually at higher temperatures reaching 0.118x..sqrt..3.2..pi../a A/sup -1/ at Tsub(N).

  17. Elastic neutron diffraction study of transforming and non-transforming single crystal ZrV2

    International Nuclear Information System (INIS)

    Bostock, J.; Wong, M.; MacVicar, M.L.A.; Levinson, M.

    1980-01-01

    The mosaic spread of single crystal ZrV 2 is unusually narrow, approx. 1' from room temperature to 130K. For non-transforming perfect single crystal the mosaic gradually increases to approx. 1.86' at 4.2K; for transforming, twinned single crystal the room temperature mosaic is maintained to 110K, then increases to 2.76' at 94K when the crystal transforms to a mixed cubic (30%) and rhombohedral state (70%). The onset of the electronic instability (approx. 100K) is accompanied by an increase in diffuse scattering background which, for the twinned crystal, peaks at the structural transformation. The electronic instability coupled to the localized lattice stress appears to be the driving mechanism for the transformation

  18. Single crystal polarized neutron diffraction study of the magnetic structure of HoFeO3.

    Science.gov (United States)

    Chatterji, T; Stunault, A; Brown, P J

    2017-09-27

    Polarised neutron diffraction measurements have been made on HoFeO 3 single crystals magnetised in both the [0 0 1] and [1 0 0] directions (Pbnm setting). The polarisation dependencies of Bragg reflection intensities were measured both with a high field of [Formula: see text] T parallel to [0 0 1] at [Formula: see text] K and with the lower field [Formula: see text] T parallel to [1 0 0] at [Formula: see text] K. A Fourier projection of magnetization induced parallel to [0 0 1], made using the hk0 reflections measured in 9 T, indicates that almost all of it is due to alignment of Ho moments. Further analysis of the asymmetries of general reflections in these data showed that although, at 70 K, 9 T applied parallel to [0 0 1] hardly perturbs the antiferromagnetic order of the Fe sublattices, it induces significant antiferromagnetic order of the Ho sublattices in the [Formula: see text] plane, with the antiferromagnetic components of moment having the same order of magnitude as the induced ferromagnetic ones. Strong intensity asymmetries measured in the low temperature [Formula: see text] structure with a lower field, 0.5 T [Formula: see text] [1 0 0] allowed the variation of the ordered components of the Ho and Fe moments to be followed. Their absolute orientations, in the [Formula: see text] domain stabilised by the field were determined relative to the distorted perovskite structure. This relationship fixes the sign of the Dzyalshinski-Moriya (D-M) interaction which leads to the weak ferromagnetism. Our results indicate that the combination of strong y-axis anisotropy of the Ho moments and Ho-Fe exchange interactions breaks the centrosymmetry of the structure and could lead to ferroelectric polarization.

  19. Strength of shock-loaded single-crystal tantalum [100] determined using in situ broadband x-ray Laue diffraction.

    Science.gov (United States)

    Comley, A J; Maddox, B R; Rudd, R E; Prisbrey, S T; Hawreliak, J A; Orlikowski, D A; Peterson, S C; Satcher, J H; Elsholz, A J; Park, H-S; Remington, B A; Bazin, N; Foster, J M; Graham, P; Park, N; Rosen, P A; Rothman, S R; Higginbotham, A; Suggit, M; Wark, J S

    2013-03-15

    The strength of shock-loaded single crystal tantalum [100] has been experimentally determined using in situ broadband x-ray Laue diffraction to measure the strain state of the compressed crystal, and elastic constants calculated from first principles. The inferred strength reaches 35 GPa at a shock pressure of 181 GPa and is in excellent agreement with a multiscale strength model [N. R. Barton et al., J. Appl. Phys. 109, 073501 (2011)], which employs a hierarchy of simulation methods over a range of length scales to calculate strength from first principles.

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

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Naresh; Kant, Rajni, E-mail: vivek-gupta2k2@hotmail.com; Gupta, Vivek K., E-mail: vivek-gupta2k2@hotmail.com [Department of Physics and Electronics, University of Jammu, Jammu Tawi - 180006 (India); Jadeja, R. N. [Department of Chemistry, Faculty of Science, The M. S. University of Baroda, Vadodara-390002 (India)

    2014-04-24

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

  1. Purification, crystallization, X-ray diffraction analysis and phasing of an engineered single-chain PvuII restriction endonuclease

    International Nuclear Information System (INIS)

    Meramveliotaki, Chrysi; Kotsifaki, Dina; Androulaki, Maria; Hountas, Athanasios; Eliopoulos, Elias; Kokkinidis, Michael

    2007-01-01

    PvuII is the first type II restriction endonuclease to be converted from its wild-type homodimeric form into an enzymatically active single-chain variant. The enzyme was crystallized and phasing was successfully performed by molecular replacement. The restriction endonuclease PvuII from Proteus vulgaris has been converted from its wild-type homodimeric form into the enzymatically active single-chain variant scPvuII by tandemly joining the two subunits through the peptide linker Gly-Ser-Gly-Gly. scPvuII, which is suitable for the development of programmed restriction endonucleases for highly specific DNA cleavage, was purified and crystallized. The crystals diffract to a resolution of 2.35 Å and belong to space group P4 2 , with unit-cell parameters a = b = 101.92, c = 100.28 Å and two molecules per asymmetric unit. Phasing was successfully performed by molecular replacement

  2. X-ray diffraction study of stacking faults in a single crystal of 2H SiC

    International Nuclear Information System (INIS)

    Pandey, D.; Krishna, P.

    1977-01-01

    The nature of random stacking faults in a heavily disordered single crystal of 2H SiC has been investigated by studying the broadening of x-ray diffraction maxima. The intensity distribution along the 10.1 reciprocal lattice row was recorded on a four-circle, computer-controlled single crystal diffractometer. The 10.1 reflections with 1 even were found to be considerably broadened showing that the stacking faults present are predominantly intrinsic faults ( both growth and deformation faults). A careful study of the half-width values of different 10.1 reflections revealed that the fault probabilities are large. Exact expressions for the diffracted intensity and the observable diffraction effects were obtained and these were then used to calculate the deformation and growth fault probabilities which were found to be 0.20 and 0.11 respectively. It is suggested that several deformation fault configurations result from a clustering of growth faults. The results obtained are compared with those obtained for 2H ZnS crystals. (author)

  3. single crystals

    Indian Academy of Sciences (India)

    2018-05-18

    May 18, 2018 ... Abstract. 4-Nitrobenzoic acid (4-NBA) single crystals were studied for their linear and nonlinear optical ... studies on the proper growth, linear and nonlinear optical ..... between the optic axes and optic sign of the biaxial crystal.

  4. Laue diffraction: The key to neutron crystallography from submillimetric-volume single crystals

    Science.gov (United States)

    Lemée-Cailleau, M.-H.; McIntyre, G. J.; Wilkinson, C.

    2005-12-01

    For several decades, chemists and physicists have been fascinated by molecular compounds rich in delocalized electrons. In the solid state these compounds may offer a very rich fan of properties: optical, conduction and dielectric, magneticldots Each state is the result of a delicate balance amongst intra- and/or intermolecular interactions which can be controlled, not just by direct chemical substitution, but also by external parameters such as temperature, pressure, continuous electric or magnetic fields, or by light. The recent evolution of this field of science towards more and more sophisticated materials makes also more and more difficult their crystal growth. While neutron scattering is an extremely powerful technique to get precise structural information, it is also often disregarded in this field because usually large single crystals are required. With the recent renaissance of Laue techniques using the very intense flux provided by the reactor of the Institut Laue-Langevin (ILL), accurate structural and/or magnetic information can be now extracted routinely from molecular crystals of volume 0.1 mm3 or smaller, with easy possibilities of high pressure (up to 3 GPa) down to 0.2 K. A general survey of these new possibilities is illustrated by an example taken from the field of low-dimensional organic complexes.

  5. Surface structure determinations of crystalline ionic thin films grown on transition metal single crystal surfaces by low energy electron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, Joel Glenn [Univ. of California, Berkeley, CA (United States)

    2000-05-01

    The surface structures of NaCl(100), LiF(100) and alpha-MgCl2(0001) adsorbed on various metal single crystals have been determined by low energy electron diffraction (LEED). Thin films of these salts were grown on metal substrates by exposing the heated metal surface to a molecular flux of salt emitted from a Knudsen cell. This method of investigating thin films of insulators (ionic salts) on a conducting substrate (metal) circumvents surface charging problems that plagued bulk studies, thereby allowing the use of electron-based techniques to characterize the surface.

  6. Crystal structures of eight mono-methyl alkanes (C26–C32 via single-crystal and powder diffraction and DFT-D optimization

    Directory of Open Access Journals (Sweden)

    Lee Brooks

    2015-09-01

    Full Text Available The crystal structures of eight mono-methyl alkanes have been determined from single-crystal or high-resolution powder X-ray diffraction using synchrotron radiation. Mono-methyl alkanes can be found on the cuticles of insects and are believed to act as recognition pheromones in some social species, e.g. ants, wasps etc. The molecules were synthesized as pure S enantiomers and are (S-9-methylpentacosane, C26H54; (S-9-methylheptacosane and (S-11-methylheptacosane, C28H58; (S-7-methylnonacosane, (S-9-methylnonacosane, (S-11-methylnonacosane and (S-13-methylnonacosane, C30H62; and (S-9-methylhentriacontane, C32H66. All crystallize in space group P21. Depending on the position of the methyl group on the carbon chain, two packing schemes are observed, in which the molecules pack together hexagonally as linear rods with terminal and side methyl groups clustering to form distinct motifs. Carbon-chain torsion angles deviate by less than 10° from the fully extended conformation, but with one packing form showing greater curvature than the other near the position of the methyl side group. The crystal structures are optimized by dispersion-corrected DFT calculations, because of the difficulties in refining accurate structural parameters from powder diffraction data from relatively poorly crystalline materials.

  7. The application of X-ray, γ-ray and neutron diffraction to the characterization of single crystal perfection

    International Nuclear Information System (INIS)

    Freund, A.; Schneider, J.R.

    1976-01-01

    The work is divided into the following three chapters: 1) diffraction by perfect and imperfect crystals, 2) experimental apparatus (describing gamma ray, X-ray and neutron diffractometers), 3) application of diffraction methods to the development of neutron monochromators. (WBU) [de

  8. 2-nitrobenzohydrazide as a potent urease inhibitor: synthesis, characterization and single crystal x-ray diffraction analysis

    International Nuclear Information System (INIS)

    Abbas, N.; Khan, I.; Hameed, S.; Batool, S.

    2018-01-01

    2-Nitrobenzohydrazide was efficiently synthesized in two steps by the esterification of 2-nitrobenzoic acid followed by the treatment with hydrazine hydrate in methanol. The structure of 2-nitrobenzohydrazide was established by modern spectro-analytical techniques including FTIR, 1H and 13C-NMR spectroscopy and unequivocally confirmed by single crystal X-ray diffraction data. 2-Nitrobenzohydrazide crystallized in orthorhombic space group P 21 21 21 with unit cell dimensions a = 4.9764(4) Å, b = 12.5280 (3) Å, c = 12.8512(1) Å, α = β = γ = 90°. A combination of N‒H…N and N‒H…O hydrogen bonds stabilized the crystal packing of 3. The synthesized compound 3 was assessed as urease inhibitor against Jack bean urease and the results revealed good inhibitory potency with an IC50 value of 4.25 ± 0.08 µM. This inhibition strength was 5-fold higher compared to the reference inhibitor thiourea (IC50 = 21.00 ± 0.11 µM). The molecular docking studies of the synthesized inhibitor 3 inside the active pocket of urease revealed several important binding interactions. (author)

  9. Accurate X-ray diffraction studies of KTiOPO{sub 4} single crystals doped with niobium

    Energy Technology Data Exchange (ETDEWEB)

    Novikova, N. E., E-mail: natnov@ns.crys.ras.ru; Sorokina, N. I.; Alekseeva, O. A.; Verin, I. A. [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Crystallography and Photonics Federal Scientific Research Center (Russian Federation); Kharitonova, E. P.; Orlova, E. I.; Voronkova, V. I. [Moscow State University, Faculty of Physics (Russian Federation)

    2017-01-15

    Single crystals of potassium titanyl phosphate doped with 4% of niobium (КТР:4%Nb) and 6% of niobium (KTP:6%Nb) are studied by accurate X-ray diffraction at room temperature. The niobium atoms are localized near the Ti1 and Ti2 atomic positions, and their positions are for the first time refined independent of the titanium atomic positions. Maps of difference electron density in the vicinity of K1 and K2 atomic positions are analyzed. It is found that in the structure of crystal КТР:4%Nb, additional positions of K atoms are located farther from the main positions and from each other than in КТР and KTP:6%Nb crystals. The nonuniform distribution of electron density found in the channels of the КТР:4%Nb structure is responsible for ~20% increase in the signal of second harmonic generation.

  10. Development of a new micro-furnace for "in situ" high-temperature single crystal X-ray diffraction measurements

    Science.gov (United States)

    Alvaro, Matteo; Angel, Ross J.; Marciano, Claudio; Zaffiro, Gabriele; Scandolo, Lorenzo; Mazzucchelli, Mattia L.; Milani, Sula; Rustioni, Greta; Domeneghetti, Chiara M.; Nestola, Fabrizio

    2015-04-01

    Several experimental methods to reliably determine elastic properties of minerals at non-ambient conditions have been developed. In particular, different techniques for generating high-pressure and high-temperature have been successfully adopted for single-crystal and powder X-ray diffraction measurements. High temperature devices for "in-situ" measurements should provide the most controlled isothermal environment as possible across the entire sample. It is intuitive that in general, thermal gradients across the sample increase as the temperature increases. Even if the small isothermal volume required for single-crystal X-ray diffraction experiments makes such phenomena almost negligible, the design of a furnace should also aim to reduce thermal gradients by including a large thermal mass that encloses the sample. However this solution often leads to complex design that results in a restricted access to reciprocal space or attenuation of the incident or diffracted intensity (with consequent reduction of the accuracy and/or precision in lattice parameter determination). Here we present a newly-developed H-shaped Pt-Pt/Rh resistance microfurnace for in-situ high-temperature single-crystal X-ray diffraction measurements. The compact design of the furnace together with the long collimator-sample-detector distance allows us to perform measurements up to 2θ = 70° with no further restrictions on any other angular movement. The microfurnace is equipped with a water cooling system that allows a constant thermal gradient to be maintained that in turn guarantees thermal stability with oscillations smaller than 5°C in the whole range of operating T of room-T to 1200°C. The furnace has been built for use with a conventional 4-circle Eulerian geometry equipped with point detector and automated with the SINGLE software (Angel and Finger 2011) that allows the effects of crystal offsets and diffractometer aberrations to be eliminated from the refined peak positions by the 8

  11. Adsorption structure of dimethyl ether on silicalite-1 zeolite determined using single-crystal X-ray diffraction

    International Nuclear Information System (INIS)

    Fujiyama, Shinjiro; Seino, Shintaro; Kamiya, Natsumi; Nishi, Koji; Yokomori, Yoshinobu

    2014-01-01

    The most stable sorption site of dimethyl ether on silicalite-1 is the sinusoidal channel. The configuration of guest molecules (linear or bent) plays an important role in determining where the stable sorption site is situated. The adsorption structures of dimethyl ether (DME) on silicalite-1 zeolite (MFI-type) are determined using single-crystal X-ray diffraction. The structure of low-loaded DME-silicalite-1 indicates that all DME molecules are located in the sinusoidal channel, which is the most stable sorption site based on the van der Waals interaction between DME and the framework. The configuration of guest molecules (linear or bent) plays an important role in determining where the stable sorption site is in the pore system of MFI-type zeolites. Bent molecules favor the sinusoidal channel, while linear molecules favor the straight channel. The contribution of DME–DME interactions is considerable in the high-loaded DME-silicalite-1 structure

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

    Science.gov (United States)

    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.

  13. Development of a large area, curved two-dimensional detector for single-crystal neutron diffraction studies

    International Nuclear Information System (INIS)

    Moon, Myung-Kook; Lee, Chang-Hee; Kim, Shin-Ae; Noda, Yukio

    2013-01-01

    A new type of two-dimensional curved position-sensitive neutron detector has been developed for a high-throughput single-crystal neutron diffractometer, which was designed to cover 110° horizontally and 56° vertically. The prototype curved detector covering 70° horizontally and 45° vertically was first developed to test the technical feasibility of the detector parameters, the internal anode and cathode structures for the curved shape, technical difficulties in the assembly procedure, and so on. Then, based on this experience, a full-scale curved detector with twice the active area of the prototype was fabricated with newly modified anode and cathode planes and optimized design parameters in terms of mechanical and electric properties. The detector was installed in a dedicated diffractometer at the ST3 beam port of the research reactor HANARO. In this paper, the fabrication and application of the prototype and a new larger-area curved position-sensitive neutron detector for single crystal diffraction is presented

  14. X-ray diffraction studies of NbTe2 single crystal

    Indian Academy of Sciences (India)

    Unknown

    X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and ... The layered structure compound, NbTe2, is one of the typical materials which lead to charge .... financial assistance to carry out this work. References. Brown B E 1966 Acta ...

  15. Anelasticity of olivine single crystals investigated by stress-reduction tests and high-angular resolution electron backscatter diffraction

    Science.gov (United States)

    Wallis, D.; Hansen, L. N.; Kempton, I.; Wilkinson, A. J.

    2017-12-01

    Geodynamic phenomena, including glacial isostatic adjustment and postseismic deformation, can involve transient deformation in response to changes in differential stress acting on mantle rocks. As such, rheological models of transient deformation are incorporated in predictions of associated processes, including sea-level rise and stress redistribution after earthquakes. However, experimental constraints on rheological models for transient deformation of mantle materials are sparse. In particular, experiments involving stress reductions have been lacking. Moreover, a material's response to a reduction in stress can provide clues to the microphysical processes controlling deformation. To constrain models of transient deformation of mantle rocks we performed stress-reduction tests on single crystals of olivine at 1250-1300°C. Mechanical and piezoelectric actuators controlled constant initial stress during creep. At various strain intervals stress was reduced near-instantaneously using the piezoelectric actuator, inducing both elastic and anelastic (time-dependent) lengthening of the samples. A range of magnitudes of stress reduction were applied, typically unloading 10-90% of the initial stress. High-angular resolution electron backscatter diffraction (HR-EBSD), based on cross-correlation of diffraction patterns, was used to map dislocation density and elastic strain distributions in the recovered samples. Magnitudes of anelastic back-strain increase with increasing magnitudes of stress reduction and show a marked increase when stress reductions exceed 50% of the initial stress, consistent with previous observations in metals and alloys. This observation is inconsistent with the Burgers rheological model commonly used to describe transient behaviour and suggests that the style of rheological behaviour depends on the magnitude of stress change. HR-EBSD maps reveal that the crystal lattices are smoothly curved and generally lack subgrain boundaries and elastic strain

  16. High pressure Raman and single crystal X-ray diffraction of the alkali/calcium carbonate, shortite

    Science.gov (United States)

    Williams, Q. C.; Vennari, C.; O'Bannon, E. F., III

    2015-12-01

    Raman and synchrotron-based single crystal x-ray diffraction data have been collected on shortite (Na2Ca2(CO3)3) up to 10 GPa at 300 K. Shortite is of geological importance due to its presence in the ground-mass of kimberlites, and the alkaline-/carbon-rich character of kimberlitic eruptions. This investigation focuses on shortite's high pressure behavior and is relevant to the behavior of alkali-carbonate systems within Earth's upper mantle. X-ray data demonstrate that shortite's symmetry remains stable at high pressures—retaining orthorhombic C crystal system (Amm2) up to 10 GPa; diffraction data show a 12% volume decrease from room pressure, and a bulk modulus of 71.0(3) GPa. These also demonstrate that the c-axis is twice as compressible as the a- and b-axes. This anisotropic compression is likely due to the orientation of the relatively stiff carbonate groups, a third of which are oriented close to the plane of the a- and b-axes, c axis compression primarily involves the compaction of the 9-fold coordinate sodium and calcium polyhedral. The two distinct carbonate sites within the unit cell give rise to two Raman symmetric stretching modes of the symmetric stretch; the carbonate group stretching vibration which is close to in plane with the a- and b-axes shifts at 3.75 cm-1/GPa as opposed to the carbonate groups which is closer to in plane with the b- and c-axes which shift at 4.25 cm-1/GPa. This furthers evidence for anisotropic compression observed using x-ray diffraction--as the carbonate in plane with the a- and b-axes is compressed, the strength of oxygen bonds along the c-axis with the cations increases, thus decreasing the pressure shift of the mode. The out of plane bending vibration shifts at -0.48 cm-1/GPa, indicating an enhanced interaction of the oxygens with the cations. The multiple in plane bending modes all shift positively, as do at the low frequency lattice modes, indicating that major changes in bonding do not occur up to 10 GPa. The data

  17. High Pressure Low Temperature X-Ray Diffraction Studies of UO2 and UN single crystals.

    Science.gov (United States)

    Antonio, Daniel; Mast, Daniel; Lavina, Barbara; Gofryk, Krzysztof

    Uranium dioxide is the most commonly used nuclear fuel material in commercial reactors, while uranium nitride also has many thermal and physical properties that make it attractive for potential use in reactors. Both have a cubic fcc lattice structure at ambient conditions and transition to antiferromagnetic order at low temperature. UO2 is a Mott insulator that orders in a complex non-collinear 3k magnetic structure at about 30 K, while UN has appreciable conductivity and orders in a simpler 1k magnetic structure below 52 K. Both compounds are characterized by strong magneto-structural interactions, understanding of which is vital for modeling their thermo-physical properties. While UO2 and UN have been extensively studied at and above room temperature, little work has been done to directly study the structure of these materials at low temperatures where magnetic interactions are dominant. In the course of our systematic studies on magneto vibrational behavior of UO2 and UN, here we present our recent results of high pressure X-Ray Diffraction (up to 35 GPa) measured below the Neel temperature using synchrotron radiation. Work supported by the Department of Energy, Office of Basic Energy Sciences, Materials Sciences, and Engineering Division.

  18. Structural characterization of Li1.2v3o8 insertion electrodes by single-crystal x-ray-diffraction

    CSIR Research Space (South Africa)

    De Picciotto, LA

    1993-08-01

    Full Text Available The crystal structures of Li1.2V3O8 and a lithiated product Li4.0V3O8 have been determined by single-crystal X-ray diffraction methods. The structure refinement of Li1.2V308 confirms that of Li1+xV3O8(x almost-equal-to 0) reported by Wadsley thirty...

  19. High-pressure single-crystal X-ray diffraction of Tl2SeO4

    International Nuclear Information System (INIS)

    Grzechnik, Andrzej; Breczewski, Tomasz; Friese, Karen

    2008-01-01

    The effect of pressure on the crystal structure of thallium selenate (Tl 2 SeO 4 ) (Pmcn, Z=4), containing the Tl + cations with electron lone pairs, has been studied with single-crystal X-ray diffraction in a diamond anvil cell up to 3.64 GPa at room temperature. No phase transition has been observed. The compressibility data are fitted by a Murnaghan equation of state with the zero-pressure bulk modulus B 0 =29(1) GPa and the unit-cell volume at ambient pressure V 0 =529.6(8) A 3 (B'=4.00). Tl 2 SeO 4 is the least compressible in the c direction, while the pressure-induced changes of the a and b lattice parameters are quite similar. These observations can be explained by different pressure effects on the nine- and 11-fold coordination polyhedra around the two non-equivalent Tl atoms. The SeO 4 2- tetrahedra are not rigid units and become more distorted. Their contribution to the compressibility is small. The effect of pressure on the isotypical oxide materials A 2 TO 4 with the β-K 2 SO 4 structure is discussed. It appears that the presence of electron lone pairs on the Tl + cation does not seem to influence the compressibility of Tl 2 SeO 4 . - Graphical abstract: Pressure dependence of normalized lattice parameters and unit-cell volumes in Tl 2 SeO 4 (Pmcn, Z=4). The solid line is the Murnaghan equation of state

  20. The accuracy of the crystal chemical parameters at high-pressure conditions from single-crystal X-ray diffraction in diamond-anvil cell

    DEFF Research Database (Denmark)

    Periotto, Benedetta

    -ray instruments. At the same time, the high-pressure experiments have benefited by the strong improvements on the high-pressure devices, in particular the diamond-anvil cell (DAC). The aim of this research project is to assess the quality of the data obtained by means of the single-crystal X-ray diffraction...... technique through the study of different mineral phases. The procedure for setting up an experiment under high-pressure conditions, using a single crystal as sample held within a DAC, are presented here with all the details of the in situ measurements at high-pressure conditions. The research project...... started with a comparison between two different DACs, in order to define the capabilities of one of the most common types of pressure device, the ETH-type DAC. Application examples of data quality analysis have been conducted on pyroxenes (NaInSi2O6, orthoenstatite MgSiO3 and LiCrSi2O6), which...

  1. High-pressure behavior of α-boron studied on single crystals by X-ray diffraction, Raman and IR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Chuvashova, Irina, E-mail: irina.chuvashova@gmail.com [Material Physics and Technology at Extreme Conditions, Laboratory of Crystallography, University of Bayreuth, D-95440 Bayreuth (Germany); Bayerisches Geoinstitut, University of Bayreuth, D-95440 Bayreuth (Germany); Bykova, Elena; Bykov, Maxim [Bayerisches Geoinstitut, University of Bayreuth, D-95440 Bayreuth (Germany); Svitlyk, Volodymyr [European Synchrotron Radiation Facility, BP 220, F-38043 Grenoble Cedex (France); Gasharova, Biliana [Institute for Photon Science and Synchrotron Radiation, Karlsruhe Institute of Technology, P.O. Box 3640, 76021 Karlsruhe (Germany); IBPT, Karlsruhe Institute of Technology, P.O. Box 3640, 76021 Karlsruhe (Germany); Mathis, Yves-Laurent [ANKA Synchrotron Radiation Facility, Karlsruhe Institute of Technology, P.O. Box 3640, 76021 Karlsruhe (Germany); IBPT, Karlsruhe Institute of Technology, P.O. Box 3640, 76021 Karlsruhe (Germany); Caracas, Razvan [CNRS, Laboratoire de Géologie de Lyon, ENS de Lyon, UCBL Lyon 1, Université de Lyon (France); Dubrovinsky, Leonid [Bayerisches Geoinstitut, University of Bayreuth, D-95440 Bayreuth (Germany); Dubrovinskaia, Natalia [Material Physics and Technology at Extreme Conditions, Laboratory of Crystallography, University of Bayreuth, D-95440 Bayreuth (Germany)

    2017-01-15

    In the present study single crystals of rhombohedral α-B were investigated under pressure to 60 GPa by means of single-crystal X-ray diffraction. The bulk modulus of α-B was found to be K=224(7) GPa (K′=3.0(3)). Measurements of interatomic distances as a function of pressure revealed that the intericosahedral two-center two-electron (2c–2e) bonds are almost as stiff as some of intraicosahedral ones. The three-center two-electron (3c–2e) intericosahedral bonds show much higher compliance compared to other bonds in α-B. The vibrational properties of α-B under pressure were investigated by Raman spectroscopy at pressures up to 160 GPa and IR spectroscopy at pressures up to 53 GPa. - Graphical abstract: The rhombohedral α-B is highly incompressible and extremely stable: it maintains its crystal structure up to 160 GPa and its intericosahedral 2e2c bonds are almost as stiff as some of intraicosahedral ones. - Highlights: • Structural stability of α-B has been investigated up to 160 GPa on single crystals. • Single-crystal x-ray diffraction reveals that α-B is highly incompressible. • Compressibility of B{sub 12} icosahedra is considerably lower than that of the bulk material. • Intericosahedral 2e2c bonds are almost as stiff as some of intraicosahedral ones.

  2. 5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

    Science.gov (United States)

    Dey, Tanusri; Ghosh, Soumen; Ghosh, Somnath; Mukherjee, Alok Kumar

    2015-07-01

    Four 5-arylidene derivatives of Meldrum's acid, 5-(4-chlorobenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (2), 5-(3-hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3), 5-(3,4-dimethoxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (4) and 5-(2,4-dimethoxy benzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5) have been synthesized and their crystal structures have been determined using single crystal X-ray diffractometry for 2, 4 and 5 and X-ray powder diffraction for 3. The nature of intermolecular interactions in 2-5 has been analyzed through Hirshfeld surfaces and 2D fingerprint plots. The DFT optimized molecular geometries in 2-5 agree closely with those obtained from the crystallographic studies. The crystal packing in 2-5 exhibits an interplay of Osbnd H⋯O, Csbnd H⋯O, Csbnd H⋯Cl and Csbnd H⋯π (arene) hydrogen bonds and π⋯π interactions, which assemble molecules into three-dimensional architecture in 2, 3 and 5 and two-dimensional framework in 4. The Hirshfeld surface analyses of 2-5, Meldrum's acid (1) and a few related 5-arylidene derivatives of Meldrum's acid retrieved from the Cambridge Structural Database (CSD) indicate that about 85% of the Hirshfeld surface area (72% in 2 where H⋯Cl contribution is about 13%) in this class of compounds are due to H⋯H, O⋯H and C⋯H contacts. The HOMO-LUMO energy gap (>2.2 eV) in 2-5 indicates a significant degree of internal charge transfer within the molecule.

  3. Single-crystal diffraction at the Extreme Conditions beamline P02.2: procedure for collecting and analyzing high-pressure single-crystal data.

    Science.gov (United States)

    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.

  4. Generation of 3.5 W of diffraction-limited green light from SHG of a single tapered diode laser in a cascade of nonlinear crystals

    DEFF Research Database (Denmark)

    Hansen, Anders Kragh; Jensen, Ole Bjarlin; Sumpf, Bernd

    2014-01-01

    Many applications, e.g., within biomedicine stand to benefit greatly from the development of diode laser-based multi- Watt efficient compact green laser sources. The low power of existing diode lasers in the green area (about 100 mW) means that the most promising approach remains nonlinear...... frequency conversion of infrared tapered diode lasers. Here, we describe the generation of 3.5 W of diffraction-limited green light from SHG of a single tapered diode laser, itself yielding 10 W at 1063 nm. This SHG is performed in single pass through a cascade of two PPMgO:LN crystals with re...... power of 3.5 W corresponds to a power enhancement greater than 2 compared to SHG in each of the crystals individually and is the highest visible output power generated by frequency conversion of a single diode laser. Such laser sources provide the necessary pump power for biophotonics applications...

  5. Thermal expansion behavior of empressite, AgTe: A structural study by means of in situ high-temperature single-crystal X-ray diffraction

    International Nuclear Information System (INIS)

    Bindi, Luca

    2009-01-01

    The crystal structure of empressite, AgTe, a rare silver telluride, has been investigated by in situ X-ray single-crystal diffraction methods within the temperature range 298-463 K. AgTe remains orthorhombic, space group Pmnb (Pnma as standard), and shows only normal thermal expansion over the entire temperature range. The unit-cell parameters show a gradual increase with the increase of temperature. Slight adjustments in the geometry of Ag-tetrahedra and in the crystal-chemical environment of tellurium atoms occur in a continuous way without abrupt structural changes. The coefficients of thermal expansion along various axes are: α a = 1.5 x 10 -5 K -1 , α b = 3.0 x 10 -5 K -1 , α c = 2.2 x 10 -5 K -1 , and the bulk thermal expansion coefficient α V is 5.4 x 10 -5 K -1 for the temperature range 298-463 K

  6. X-ray and neutron single crystal diffraction on (NH4)3H(SO4)2. II. Refinement of crystal structure of phase II at room temperature

    International Nuclear Information System (INIS)

    Reehuis, M.; Wozniak, K.; Dominiak, P.; Smirnov, L.S.; Natkaniec, I.; Baranov, A.I.; Dolbinina, V.V.

    2006-01-01

    The (NH 4 ) 3 H(SO 4 ) 2 is of special interest due to the possible influence of ammonium ions on a series of phase transitions: I => II => III => IV => V => VII. Earlier, the X-ray single crystal diffraction study of phase II of (NH 4 ) 3 H(SO 4 ) 2 showed that the crystal structure of this compound has two crystallographically independent groups of ammonium ions NH 4 (1) and NH 4 (2), but orientational positions of these ammonium ions were not determined exactly. The refinement of NH 4 (1) and NH 4 (2) orientational positions in phase II is carried out with the help of the X-ray and neutron single crystal diffraction study. The analyses of differential Fourier maps of electron charge density and nuclear density point out the possibility of disordering of NH 4 (2) ammonium ions

  7. Characterization of CuCl quantum dots grown in NaCl single crystals via optical measurements, X-ray diffraction, and transmission electron microscopy

    Science.gov (United States)

    Miyajima, Kensuke; Akatsu, Tatsuro; Itoh, Ken

    2018-05-01

    We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs) embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and transmission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work will play an important role in progressing the study of optical phenomena originating from assembled semiconductor QDs.

  8. Crystal structure investigations of ZrAsxSey (x>y, x+y≤2) by single crystal neutron diffraction at 300 K, 25 K and 2.3 K

    International Nuclear Information System (INIS)

    Niewa, Rainer; Czulucki, Andreas; Schmidt, Marcus; Auffermann, Gudrun; Cichorek, Tomasz; Meven, Martin; Pedersen, Bjoern; Steglich, Frank; Kniep, Ruediger

    2010-01-01

    Large single crystals of ZrAs x Se y (x>y, x+y≤2, PbFCl type of structure, space group P4/nmm) were grown by Chemical Transport. Structural details were studied by single crystal neutron diffraction techniques at various temperatures. One single crystal specimen with chemical composition ZrAs 1.595(3) Se 0.393(1) was studied at ambient temperature (R1=5.10 %, wR2=13.18 %), and a second crystal with composition ZrAs 1.420(3) Se 0.560(1) was investigated at 25 K (R1=2.70%, wR2=5.70 %) and 2.3 K (R1=2.30 %, wR2=4.70 %), respectively. The chemical compositions of the crystals under investigation were determined by wavelength dispersive X-ray spectroscopy. The quantification of trace elements was carried out by Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry. According to the crystal structure refinements the crystallographic 2a site is occupied by As, together with a significant amount of vacancies. One of the 2c sites is fully occupied by As and Se (random distribution). With respect to the fractional coordinates of the atoms, the crystal structure determinations based on the data obtained at 25.0 K and 2.3 K did not show significant deviations from ambient temperature results. The temperature dependence of the displacement parameters indicates a static displacement of As on the 2a sites (located on the (0 0 1) planes) for all temperatures. No indications for any occupation of interstitial sites or the presence of vacancies on the Zr (2a) site were found. - Graphical abstract: Large single crystals of ZrAs x Se y grown by Chemical Transport to study structural details as the As-Se order scheme by single crystal neutron diffraction.

  9. X-ray and neutron single-crystal diffraction on [Rbx(NH4)1-x]3H(SO4)2. I. Refinement of crystal structure of phase II with x=0.11 at 300 K

    International Nuclear Information System (INIS)

    Loose, A.; Wozniak, K.; Dominiak, P.; Smirnov, L.S.; Natkaniec, I.; Frontas'eva, M.V.; Pomyakushina, E.V.; Baranov, A.I.; Dolbinina, V.V

    2006-01-01

    The study of [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals by X-ray single-crystal diffraction is known up to now only for x=0.57 at the temperatures 293 and 180 K. The crystal structures at these temperatures as was determined [1] belong to monoclinic phase II (C2/c sp. gr., Z=4). In accordance with this work, ammonium ions should be considered as deformed tetrahedra. Monoclinic phase II on the x-T phase diagram of [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals, which has earlier been determined by the dielectric spectroscopy, is stabilized below room temperature if Rb concentration exceeds 9%. The presented results of X-ray and neutron single-crystal diffraction of the [Rb 0.11 (NH 4 ) 0.89 ] 3 H(SO 4 ) 2 mixed crystal at T= 300 K show that ammonium ions could be considered as regular tetrahedra

  10. Redetermination of eveite, Mn2AsO4(OH, based on single-crystal X-ray diffraction data

    Directory of Open Access Journals (Sweden)

    Yongbo W. Yang

    2011-12-01

    Full Text Available The crystal structure of eveite, ideally Mn2(AsO4(OH [dimanganese(II arsenate(V hydroxide], was refined from a single crystal selected from a co-type sample from Långban, Filipstad, Varmland, Sweden. Eveite, dimorphic with sarkinite, is structurally analogous with the important rock-forming mineral andalusite, Al2OSiO4, and belongs to the libethenite group. Its structure consists of chains of edge-sharing distorted [MnO4(OH2] octahedra (..2 symmetry extending parallel to [001]. These chains are cross-linked by isolated AsO4 tetrahedra (..m symmetry through corner-sharing, forming channels in which dimers of edge-sharing [MnO4(OH] trigonal bipyramids (..m symmetry are located. In contrast to the previous refinement from Weissenberg photographic data [Moore & Smyth (1968. Am. Mineral. 53, 1841–1845], all non-H atoms were refined with anisotropic displacement parameters and the H atom was located. The distance of the donor and acceptor O atoms involved in hydrogen bonding is in agreement with Raman spectroscopic data. Examination of the Raman spectra for arsenate minerals in the libethenite group reveals that the position of the peak originating from the O—H stretching vibration shifts to lower wavenumbers from eveite, to adamite, zincolivenite, and olivenite.

  11. Order-disorder-reorder process in thermally treated dolomite samples: a combined powder and single-crystal X-ray diffraction study

    Science.gov (United States)

    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.

  12. Crystal diffraction lens for medical imaging

    International Nuclear Information System (INIS)

    Smither, R. K.; Roa, D. E.

    2000-01-01

    A crystal diffraction lens for focusing energetic gamma rays has been developed at Argonne National Laboratory for use in medical imaging of radioactivity in the human body. A common method for locating possible cancerous growths in the body is to inject radioactivity into the blood stream of the patient and then look for any concentration of radioactivity that could be associated with the fast growing cancer cells. Often there are borderline indications of possible cancers that could be due to statistical functions in the measured counting rates. In order to determine if these indications are false or real, one must resort to surgical means and take tissue samples in the suspect area. They are developing a system of crystal diffraction lenses that will be incorporated into a 3-D imaging system with better sensitivity (factors of 10 to 100) and better spatial resolution (a few mm in both vertical and horizontal directions) than most systems presently in use. The use of this new imaging system will allow one to eliminate 90% of the false indications and both locate and determine the size of the cancer with mm precision. The lens consists of 900 single crystals of copper, 4 mm x 4 mm on a side and 2--4 mm thick, mounted in 13 concentric rings

  13. A combined temperature-dependent electron and single-crystal X-ray diffraction study of the fresnoite compound Rb2V4+V25+O8

    International Nuclear Information System (INIS)

    Withers, R.L.; Hoeche, Thomas; Liu Yun; Esmaeilzadeh, Saeid; Keding, Ralf; Sales, Brian

    2004-01-01

    High-purity Rb 2 V 3 O 8 has been grown and temperature-dependent electron and single-crystal X-ray diffraction used to carefully investigate its fresnoite-type reciprocal lattice. In contrast to other recently investigated representatives of the fresnoite family of compounds, Rb 2 V 3 O 8 is not incommensurately modulated with an incommensurate basal plane primary modulation wave vector given by q∼0.3 *. A careful low-temperature electron diffraction study has, however, revealed the existence of weak incommensurate satellite reflections characterized by the primitive primary modulation wave vector q 1 ∼0.16c*. The reciprocal space positioning of these incommensurate satellite reflections, the overall (3+1)-d superspace group symmetry, as well as the shapes of the refined displacement ellipsoids determined from single-crystal XRD refinement, are all consistent with their arising from a distinct type of condensed rigid unit modes (RUMs) of distortion of the Rb 2 V 3 O 8 parent structure

  14. Slit and phase grating diffraction with a double crystal diffractometer

    International Nuclear Information System (INIS)

    Treimer, Wolfgang; Hilger, Andre; Strobl, Markus

    2006-01-01

    The lateral coherence properties of a neutron beam (λ=0.5248nm) in a double crystal diffractometer (DCD) were studied by means of single slit diffraction and by diffraction by different perfect Silicon phase gratings. Perfect agreements were found for the lateral coherence length measured with the slit and for the one determined by Silicon phase gratings, however, some peculiarities are still present

  15. Pressure-induced phase transitions in organic molecular crystals: a combination of x-ray single-crystal and powder diffraction, raman and IR-spectroscopy

    International Nuclear Information System (INIS)

    Boldyreva, E V; Goryainov, S V; Seryotkin, Y V; Kolesnik, E N; Shakhtshneider, T P; Ivashevskaya, S N; Drebushchak, T N; Sowa, H; Ahsbahs, H; Chernyshev, V V; Dmitriev, V P

    2008-01-01

    The contribution summarizes the results of recent studies of phase transitions induced by high pressure in a number of molecular organic crystals, such as polymorphs of paracetamol, chlorpropamide, polymorphs of glycine, L- and DL-serine, β-alanine. The main attention is paid to the following topics: (1) Reversible / irreversible transformations; (2) Different behavior of single crystals / powders; (3) The role of pressure-transmitting liquid; (4) The role of the kinetic factors: phase transitions on decompression, or after a long storage at a selected pressure; (5) Isosymmetric phase transitions; (6) The role of the changes in the hydrogen bond networks / intramolecular conformational changes in the phase transitions; (7) Superstructures / nanostructures formed as a result of pressure-induced phase transitions

  16. Pressure-induced phase transitions in organic molecular crystals: a combination of x-ray single-crystal and powder diffraction, raman and IR-spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Boldyreva, E V; Goryainov, S V; Seryotkin, Y V; Kolesnik, E N; Shakhtshneider, T P; Ivashevskaya, S N; Drebushchak, T N [Research and Education Center ' Molecular Design and Ecologically Safe Technologies' , REC-008, Novosibirsk State University (Russian Federation); Sowa, H [Goettingen University (Germany); Ahsbahs, H; Chernyshev, V V [Marburg University (Germany); Dmitriev, V P [Swiss-Norwegian Beamline ESRF, Grenoble (France)], E-mail: boldyrev@nsu.ru

    2008-07-15

    The contribution summarizes the results of recent studies of phase transitions induced by high pressure in a number of molecular organic crystals, such as polymorphs of paracetamol, chlorpropamide, polymorphs of glycine, L- and DL-serine, {beta}-alanine. The main attention is paid to the following topics: (1) Reversible / irreversible transformations; (2) Different behavior of single crystals / powders; (3) The role of pressure-transmitting liquid; (4) The role of the kinetic factors: phase transitions on decompression, or after a long storage at a selected pressure; (5) Isosymmetric phase transitions; (6) The role of the changes in the hydrogen bond networks / intramolecular conformational changes in the phase transitions; (7) Superstructures / nanostructures formed as a result of pressure-induced phase transitions.

  17. Hybrid Powder - Single Crystal X-Ray Diffraction Instrument for Planetary Mineralogical Analysis of Unprepared Samples, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — We propose to develop a planetary exploration XRD/XRF instrument based on a hybrid diffraction approach that complements powder XRD analysis, similar to that of the...

  18. Thermal expansion behavior of empressite, AgTe: A structural study by means of in situ high-temperature single-crystal X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Bindi, Luca [Museo di Storia Naturale, sez. di Mineralogia, Universita di Firenze, Via La Pira 4, I-50121 Firenze (Italy)], E-mail: luca.bindi@unifi.it

    2009-04-03

    The crystal structure of empressite, AgTe, a rare silver telluride, has been investigated by in situ X-ray single-crystal diffraction methods within the temperature range 298-463 K. AgTe remains orthorhombic, space group Pmnb (Pnma as standard), and shows only normal thermal expansion over the entire temperature range. The unit-cell parameters show a gradual increase with the increase of temperature. Slight adjustments in the geometry of Ag-tetrahedra and in the crystal-chemical environment of tellurium atoms occur in a continuous way without abrupt structural changes. The coefficients of thermal expansion along various axes are: {alpha}{sub a} = 1.5 x 10{sup -5} K{sup -1}, {alpha}{sub b} = 3.0 x 10{sup -5} K{sup -1}, {alpha}{sub c} = 2.2 x 10{sup -5} K{sup -1}, and the bulk thermal expansion coefficient {alpha}{sub V} is 5.4 x 10{sup -5} K{sup -1} for the temperature range 298-463 K.

  19. High-pressure single-crystal neutron diffraction (to 20 kbar) using a pulsed source: Preliminary investigation of Tl3PSe4

    International Nuclear Information System (INIS)

    Alkire, R.W.; Larson, A.C.; Vergamini, P.J.; Schirber, J.E.; Morosin, B.

    1985-01-01

    A new technique is described for performing high-pressure single-crystal neutron diffraction [up to 20 kbar (2GPa) at room temperature], using a BeCu pressure cell, an area detector and the Los Alamos National Laboratory pulsed neutron source. Success of this method depends on the increase in information available with a multi-wavelength pulse neutron source, a novel orientation of a cylindrically symmetric pressure cell with its axis coincident with the neutron beam and a specific crystal orientation within the pressure cell. Bragg scattering from the pressure cell is avoided and background for a given 2theta is constant. For a crystal of orthorhombic or higher symmetry oriented with the incident beam passing midway between the major lattice vectors, it will be possible to refine a complete three-dimensional structure with data collected from only one pressure loading. Preliminary investigations of Tl 3 PSe 4 lattice parameters (space group Pcmn) at 15(1)kbar yielded linear compressibilities (. 1000 in kbar -1 ) of Ksub(a) = 1.05(8), Ksub(b) = 1.50(10), Ksub(c) = 1.20(8). The anisotropic compressibility is explained by examination of the ambient-pressure room-temperature structure. (orig.)

  20. Intergrown new zeolite beta polymorphs with interconnected 12-ring channels solved by combining electron crystallography and single-crystal X-ray diffraction

    KAUST Repository

    Yu, Zhengbao

    2012-10-09

    Two new polymorphs of zeolite beta, denoted as SU-78A and SU-78B, were synthesized by employing dicyclohexylammonium hydroxides as organic structure-directing agents. The structure was solved by combining transmission electron microscopy and single-crystal X-ray diffraction. SU-78 is an intergrowth of SU-78A and SU-78B and contains interconnected 12-ring channels in three directions. The two polymorphs are built from the same building layer, similar to that for the zeolite beta family. The layer stacking in SU-78, however, is different from those in zeolite beta polymorph A, B, and C, showing new zeolite framework topologies. SU-78 is thermally stable up to 600 °C. © 2012 American Chemical Society.

  1. Single-crystal X-ray diffraction study of SrGeO3 high-pressure perovskite phase at 100 K

    Science.gov (United States)

    Nakatsuka, Akihiko; Arima, Hiroshi; Ohtaka, Osamu; Fujiwara, Keiko; Yoshiasa, Akira

    2017-10-01

    Single-crystal X-ray diffraction study of SrGeO3 perovskite (cubic; space group Pmɜ¯m) synthesized at 6 GPa and 1223 K was conducted at a low temperature of 100 K. The residual electron density revealed the presence of the bonding electron at the center of the Ge-O bond, in accordance with our previous conclusion that the Ge-O bond is strongly covalent. From comparison with our previous structure-refinement result at 296 K, the mean square displacement (MSD) of the O atom in the direction of the Ge-O bond is suggested to exhibit no significant temperature dependence, in contrast to that in the direction perpendicular to the bond. Thus, the strong covalency of the Ge-O bond can have a large influence on the temperature dependence of thermal vibration of the O atom.

  2. Structural characterization of framework-gas interactions in the metal-organic framework Co2(dobdc) by in situ single-crystal X-ray diffraction.

    Science.gov (United States)

    Gonzalez, Miguel I; Mason, Jarad A; Bloch, Eric D; Teat, Simon J; Gagnon, Kevin J; Morrison, Gregory Y; Queen, Wendy L; Long, Jeffrey R

    2017-06-01

    The crystallographic characterization of framework-guest interactions in metal-organic frameworks allows the location of guest binding sites and provides meaningful information on the nature of these interactions, enabling the correlation of structure with adsorption behavior. Here, techniques developed for in situ single-crystal X-ray diffraction experiments on porous crystals have enabled the direct observation of CO, CH 4 , N 2 , O 2 , Ar, and P 4 adsorption in Co 2 (dobdc) (dobdc 4- = 2,5-dioxido-1,4-benzenedicarboxylate), a metal-organic framework bearing coordinatively unsaturated cobalt(ii) sites. All these molecules exhibit such weak interactions with the high-spin cobalt(ii) sites in the framework that no analogous molecular structures exist, demonstrating the utility of metal-organic frameworks as crystalline matrices for the isolation and structural determination of unstable species. Notably, the Co-CH 4 and Co-Ar interactions observed in Co 2 (dobdc) represent, to the best of our knowledge, the first single-crystal structure determination of a metal-CH 4 interaction and the first crystallographically characterized metal-Ar interaction. Analysis of low-pressure gas adsorption isotherms confirms that these gases exhibit mainly physisorptive interactions with the cobalt(ii) sites in Co 2 (dobdc), with differential enthalpies of adsorption as weak as -17(1) kJ mol -1 (for Ar). Moreover, the structures of Co 2 (dobdc)·3.8N 2 , Co 2 (dobdc)·5.9O 2 , and Co 2 (dobdc)·2.0Ar reveal the location of secondary (N 2 , O 2 , and Ar) and tertiary (O 2 ) binding sites in Co 2 (dobdc), while high-pressure CO 2 , CO, CH 4 , N 2 , and Ar adsorption isotherms show that these binding sites become more relevant at elevated pressures.

  3. Aspherical-atom modeling of coordination compounds by single-crystal X-ray diffraction allows the correct metal atom to be identified.

    Science.gov (United States)

    Dittrich, Birger; Wandtke, Claudia M; Meents, Alke; Pröpper, Kevin; Mondal, Kartik Chandra; Samuel, Prinson P; Amin Sk, Nurul; Singh, Amit Pratap; Roesky, Herbert W; Sidhu, Navdeep

    2015-02-02

    Single-crystal X-ray diffraction (XRD) is often considered the gold standard in analytical chemistry, as it allows element identification as well as determination of atom connectivity and the solid-state structure of completely unknown samples. Element assignment is based on the number of electrons of an atom, so that a distinction of neighboring heavier elements in the periodic table by XRD is often difficult. A computationally efficient procedure for aspherical-atom least-squares refinement of conventional diffraction data of organometallic compounds is proposed. The iterative procedure is conceptually similar to Hirshfeld-atom refinement (Acta Crystallogr. Sect. A- 2008, 64, 383-393; IUCrJ. 2014, 1,61-79), but it relies on tabulated invariom scattering factors (Acta Crystallogr. Sect. B- 2013, 69, 91-104) and the Hansen/Coppens multipole model; disordered structures can be handled as well. Five linear-coordinate 3d metal complexes, for which the wrong element is found if standard independent-atom model scattering factors are relied upon, are studied, and it is shown that only aspherical-atom scattering factors allow a reliable assignment. The influence of anomalous dispersion in identifying the correct element is investigated and discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Lattice collapse and quenching of magnetism in CaFe2As2 under pressure: A single-crystal neutron and x-ray diffraction investigation

    International Nuclear Information System (INIS)

    Goldman, A.I.; Kreyssig, A.; Prokes, K.; Pratt, D.K.; Argyriou, D.N.; Lynn, J.W.; Nandi, S.; Kimber, S.A.J.; Chen, Y.; Lee, Y.B.; Samolyuk, G.; Leao, J.B.; Poulton, S.J.; Bud'ko, S.L.; Ni, N.; Canfield, P.C.; Harmon, B.N.; McQueeney, R.J.

    2009-01-01

    Single-crystal neutron and high-energy x-ray diffraction measurements have identified the phase lines corresponding to transitions among the ambient-pressure paramagnetic tetragonal (T), the antiferromagnetic orthorhombic (O), and the nonmagnetic collapsed tetragonal (cT) phases of CaFe 2 As 2 . We find no evidence of additional structures for pressures of up to 2.5 GPa (at 300 K). Both the T-cT and O-cT transitions exhibit significant hysteresis effects, and we demonstrate that coexistence of the O and cT phases can occur if a nonhydrostatic component of pressure is present. Measurements of the magnetic diffraction peaks show no change in the magnetic structure or ordered moment as a function of pressure in the O phase, and we find no evidence of magnetic ordering in the cT phase. Band-structure calculations show that the transition into the cT phase results in a strong decrease in the iron 3d density of states at the Fermi energy, consistent with a loss of the magnetic moment.

  5. An in-situ X-ray diffraction study on the electrochemical formation of PtZn alloys on Pt(1 1 1) single crystal electrode

    Energy Technology Data Exchange (ETDEWEB)

    Drnec, J., E-mail: drnec@esrf.fr [ESRF, Grenoble (France); Bizzotto, D. [Department of Chemistry, AMPEL, University of British Columbia, Vancouver, BC (Canada); Carlà, F. [ESRF, Grenoble (France); Fiala, R. [Charles University, Faculty of Mathematics and Physics, Prague (Czech Republic); Sode, A. [Ruhr-Universität Bochum, Bochum (Germany); Balmes, O.; Detlefs, B.; Dufrane, T. [ESRF, Grenoble (France); Felici, R., E-mail: felici@esrf.fr [ESRF, Grenoble (France)

    2015-11-01

    Highlights: • PtZn electrochemical alloying is observed on single crystal Pt electrodes. • In-situ X-ray characterization during alloy formation and dissolution is provided. • Structural model of the surface during alloying and dissolution is discussed. • X-ray based techniques can be used in in-operando studies of bimetallic fuel cell catalysts. - Abstract: The electrochemical formation and dissolution of the oxygen reduction reaction (ORR) PtZn catalyst on Pt(1 1 1) surface is followed by in-situ X-ray diffraction (XRD) and X-ray reflectivity (XRR) measurements. When the crystalline Pt surface is polarized to sufficiently negative potential values, with respect to an Ag/AgCl|KCl reference electrode, the electrodeposited zinc atoms diffuse into the bulk and characteristic features are observed in the X-ray patterns. The surface structure and composition during deposition and dissolution is determined from analysis of XRR curves and measurements of crystal truncation rods. Thin Zn-rich surface layer is present during the alloy formation while a Zn-depleted layer forms during dissolution.

  6. A Single-Crystal Neutron Diffraction Study on Magnetic Structure of the Quasi-One-Dimensional Antiferromagnet SrCo_2V_2O_8

    International Nuclear Information System (INIS)

    Liu Juan-Juan; Wang Jin-Chen; Luo Wei; Sheng Jie-Ming; Bao Wei; He Zhang-Zhen; Danilkin, S. A.

    2016-01-01

    The magnetic structure of the spin-chain antiferromagnet SrCo_2V2O_8 is determined by single-crystal neutron diffraction experiment. The system undergoes a long-range magnetic order below the critical temperature T_N = 4.96 K. The moment of 2.16μ_B per Co at 1.6 K in the screw chain running along the c axis alternates in the c axis. The moments of neighboring screw chains are arranged antiferromagnetically along one in-plane axis and ferromagnetically along the other in-plane axis. This magnetic configuration breaks the four-fold symmetry of the tetragonal crystal structure and leads to two equally populated magnetic twins with the antiferromagnetic vector in the a or b axis. The very similar magnetic state to the isostructural BaCo_2V_2O_8 warrants SrCo_2V_2O_8 as another interesting half-integer spin-chain antiferromagnet for investigation on quantum antiferromagnetism. (paper)

  7. Preparation of TiC single crystals

    International Nuclear Information System (INIS)

    Scheerer, B.; Fink, J.; Reichardt, W.

    1975-07-01

    TiC single crystals were prepared by vertical zone melting for measurements of the phonon dispersion by inelastic neutron scattering. The influence of the starting material and of the growing conditions on the growth of the crystal were studied. The crystals were characterized by chemical methods, EMX and neutron diffraction. It was possible to grow single crystals with a volume of up to 0.6 cm 3 and mosaic spread of less then 0.4 0 . (orig.) [de

  8. Neutron diffraction on a large block mosaic crystal

    International Nuclear Information System (INIS)

    Kim Chir Sen; Nitts, V.V.

    1985-01-01

    The neutron diffraction by the mosaic single crystal with size of crystallites sufficient to achieve the primary extinction saturation is considered. Two cases where the proportionality between the reflection intensity and the structure amplitude is performed are analysed. Such a dependence is convenient for structure investigations. The difficulties connected with the accounting of the extinction are eliminated considerably

  9. Single Hit Energy-resolved Laue Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Patel, Shamim; Suggit, Matthew J.; Stubley, Paul G.; Ciricosta, Orlando; Wark, Justin S.; Higginbotham, Andrew [Clarendon Laboratory, Department of Physics, University of Oxford, Parks Road, Oxford OX1 3PU (United Kingdom); Hawreliak, James A.; Collins, Gilbert W.; Eggert, Jon H. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Comley, Andrew J.; Foster, John M. [Atomic Weapons Establishment, Aldermaston, Reading RG7 4PR (United Kingdom)

    2015-05-15

    In situ white light Laue diffraction has been successfully used to interrogate the structure of single crystal materials undergoing rapid (nanosecond) dynamic compression up to megabar pressures. However, information on strain state accessible via this technique is limited, reducing its applicability for a range of applications. We present an extension to the existing Laue diffraction platform in which we record the photon energy of a subset of diffraction peaks. This allows for a measurement of the longitudinal and transverse strains in situ during compression. Consequently, we demonstrate measurement of volumetric compression of the unit cell, in addition to the limited aspect ratio information accessible in conventional white light Laue. We present preliminary results for silicon, where only an elastic strain is observed. VISAR measurements show the presence of a two wave structure and measurements show that material downstream of the second wave does not contribute to the observed diffraction peaks, supporting the idea that this material may be highly disordered, or has undergone large scale rotation.

  10. Single Hit Energy-resolved Laue Diffraction

    International Nuclear Information System (INIS)

    Patel, Shamim; Suggit, Matthew J.; Stubley, Paul G.; Ciricosta, Orlando; Wark, Justin S.; Higginbotham, Andrew; Hawreliak, James A.; Collins, Gilbert W.; Eggert, Jon H.; Comley, Andrew J.; Foster, John M.

    2015-01-01

    In situ white light Laue diffraction has been successfully used to interrogate the structure of single crystal materials undergoing rapid (nanosecond) dynamic compression up to megabar pressures. However, information on strain state accessible via this technique is limited, reducing its applicability for a range of applications. We present an extension to the existing Laue diffraction platform in which we record the photon energy of a subset of diffraction peaks. This allows for a measurement of the longitudinal and transverse strains in situ during compression. Consequently, we demonstrate measurement of volumetric compression of the unit cell, in addition to the limited aspect ratio information accessible in conventional white light Laue. We present preliminary results for silicon, where only an elastic strain is observed. VISAR measurements show the presence of a two wave structure and measurements show that material downstream of the second wave does not contribute to the observed diffraction peaks, supporting the idea that this material may be highly disordered, or has undergone large scale rotation

  11. Laser diffraction analysis of colloidal crystals

    Energy Technology Data Exchange (ETDEWEB)

    Sogami, Ikuo S.; Shinohara, Tadatomi; Yoshiyama, Tsuyoshi [Kyoto Sangyo Univ., Department of Physics, Kyoto (Japan)

    2001-10-01

    Laser diffraction analysis is made on crystallization in salt-free aqueous suspensions of highly-charged colloidal particles for semi-dilute specimens of concentration 0.1-10.0 vol%. Kossel diffraction patterns which represent faithfully accurate information on lattice symmetries in the suspensions enable us to investigate the time evolution of colloidal crystals. The results show that the crystallization proceeds by way of the following intermediate phase transitions: two-dimensional hcp structure {yields} random layer structure {yields} layer structure with one sliding degree of freedom {yields} stacking disorder structure {yields} stacking structure with multivariant periodicity {yields} fcc twin structure with twin plane (111) {yields} normal fcc structure {yields} bcc twin structure with twin plane (11-bar2) or (1-bar12) {yields} normal bcc structure. For concentrated suspensions (>2 vol %), the phase transition ceases to proceed at the normal fcc structure. (author)

  12. Laser diffraction analysis of colloidal crystals

    International Nuclear Information System (INIS)

    Sogami, Ikuo S.; Shinohara, Tadatomi; Yoshiyama, Tsuyoshi

    2001-01-01

    Laser diffraction analysis is made on crystallization in salt-free aqueous suspensions of highly-charged colloidal particles for semi-dilute specimens of concentration 0.1-10.0 vol%. Kossel diffraction patterns which represent faithfully accurate information on lattice symmetries in the suspensions enable us to investigate the time evolution of colloidal crystals. The results show that the crystallization proceeds by way of the following intermediate phase transitions: two-dimensional hcp structure → random layer structure → layer structure with one sliding degree of freedom → stacking disorder structure → stacking structure with multivariant periodicity → fcc twin structure with twin plane (111) → normal fcc structure → bcc twin structure with twin plane (11-bar2) or (1-bar12) → normal bcc structure. For concentrated suspensions (>2 vol %), the phase transition ceases to proceed at the normal fcc structure. (author)

  13. Neutron diffraction and magnetization studies of Tb0.5Er0.5 single crystal in an external magnetic field

    International Nuclear Information System (INIS)

    Kosugi, T.; Yamamoto, N.

    1999-01-01

    Complete text of publication follows. The rare earth Tb 0.5 Er 0.5 alloy exhibits a tilted helix at low temperatures [1]. However, the magnetic structures of Tb 0.5 Er 0.5 and the magnetization processes of the tilted helix are not clear. Neutron diffraction experiments in external magnetic fields and magnetization measurements of Tb 0.5 Er 0.5 single crystal have been performed. At zero magnetic field, the Tb 0.5 Er 0.5 alloy exhibited a normal helix below 170 K, a bunching normal helix below about 28 K, and finally a bunching tilted helix below about 25 K. Below about 60 K, the helical pitch 30 deg showed a lock-in feature. The magnetization measurements at low temperatures showed a four-step magnetic transition. The results are presented as a magnetic field-temperature (H-T) phase diagram. (author) [1] H. Fujii et al., J. Phys. Soc. Jpn. 50 (1981) 2939

  14. Fermi surface of a disordered Cu-Al -alloy single crystal studied by high-resolution Compton scattering and electron diffraction

    Science.gov (United States)

    Kwiatkowska, J.; Maniawski, F.; Matsumoto, I.; Kawata, H.; Shiotani, N.; Lityńska, L.; Kaprzyk, S.; Bansil, A.

    2004-08-01

    We have measured high resolution Compton scattering profiles for momentum transfer along a series of 28 independent directions from Cu0.842Al0.158 disordered alloy single crystals with normals to the surfaces oriented along the [100], [110], and [111] directions. The experimental spectra are interpreted via parallel first-principles KKR-CPA (Korringa-Kohn-Rostoker coherent-potential approximation) computations of these directional profiles. The Fermi surface determined by inverting the Compton data is found to be in good agreement with the KKR-CPA predictions. An electron diffraction study of the present Cu0.842Al0.158 sample is additionally undertaken to gain insight into short-range ordering effects. The scattering pattern displays not only the familiar diffuse scattering peaks, but also shows the presence of weak streaks interconnecting the four diffuse scattering spots around the (110) reciprocal lattice points. This study provides a comprehensive picture of the evolution of the shape of the Fermi surface of Cu with the addition of Al . Our results are consistent with the notion that Fermi surface nesting is an important factor in driving short-range ordering effects in disordered alloys.

  15. In Situ Neutron Diffraction Analyzing Stress-Induced Phase Transformation and Martensite Elasticity in [001]-Oriented Co49Ni21Ga30 Shape Memory Alloy Single Crystals

    Science.gov (United States)

    Reul, A.; Lauhoff, C.; Krooß, P.; Gutmann, M. J.; Kadletz, P. M.; Chumlyakov, Y. I.; Niendorf, T.; Schmahl, W. W.

    2018-02-01

    Recent studies demonstrated excellent pseudoelastic behavior and cyclic stability under compressive loads in [001]-oriented Co-Ni-Ga high-temperature shape memory alloys (HT-SMAs). A narrow stress hysteresis was related to suppression of detwinning at RT and low defect formation during phase transformation due to the absence of a favorable slip system. Eventually, this behavior makes Co-Ni-Ga HT-SMAs promising candidates for several industrial applications. However, deformation behavior of Co-Ni-Ga has only been studied in the range of theoretical transformation strain in depth so far. Thus, the current study focuses not only on the activity of elementary deformation mechanisms in the pseudoelastic regime up to maximum theoretical transformation strains but far beyond. It is shown that the martensite phase is able to withstand about 5% elastic strain, which significantly increases the overall deformation capability of this alloy system. In situ neutron diffraction experiments were carried out using a newly installed testing setup on Co-Ni-Ga single crystals in order to reveal the nature of the stress-strain response seen in the deformation curves up to 10% macroscopic strain.

  16. Variable-temperature single-crystal X-ray diffraction study of tetragonal and cubic perovskite-type barium titanate phases.

    Science.gov (United States)

    Nakatani, Tomotaka; Yoshiasa, Akira; Nakatsuka, Akihiko; Hiratoko, Tatsuya; Mashimo, Tsutomu; Okube, Maki; Sasaki, Satoshi

    2016-02-01

    A variable-temperature single-crystal X-ray diffraction study of a synthetic BaTiO3 perovskite has been performed over the temperature range 298-778 K. A transition from a tetragonal (P4mm) to a cubic (Pm3m) phase has been revealed near 413 K. In the non-centrosymmetric P4mm symmetry group, both Ti and O atoms are displaced along the c-axis in opposite directions with regard to the Ba position fixed at the origin, so that Ti(4+) and Ba(2+) cations occupy off-center positions in the TiO6 and BaO12 polyhedra, respectively. Smooth temperature-dependent changes of the atomic coordinates become discontinuous with the phase transition. Our observations imply that the cations remain off-center even in the high-temperature cubic phase. The temperature dependence of the mean-square displacements of Ti in the cubic phase includes a significant static component which means that Ti atoms are statistically distributed in the off-center positions.

  17. Polarized single crystal neutron diffraction study of the zero-magnetization ferromagnet Sm1 -xGdxAl2 (x =0.024 )

    Science.gov (United States)

    Chatterji, T.; Stunault, A.; Brown, P. J.

    2018-02-01

    We have determined the temperature evolution of the spin and orbital moments in the zero-magnetization ferromagnet Sm1 -xGdxAl2 (x = 0.024) by combining polarized and unpolarized single crystal neutron diffraction data. The sensitivity of the polarized neutron technique has allowed the moment values to be determined with a precision of ≈0.1 μB . Our results clearly demonstrate that, when magnetized by a field of 8 T, the spin and orbital moments in Sm1 -xGdxAl2 are oppositely directed, so that the net magnetization is very small. Below 60 K the contributions from spin and orbital motions are both about 2 μB , with that due to orbital motion being slightly larger than that due to spin. Between 60 and 65 K the contributions of each to the magnetization fall rapidly and change sign at Tcomp ≈67 K , above which the aligned moments recover but with the orbital magnetization still slightly higher than the spin one. These results imply that above Tcomp the small resultant magnetization of the Sm3 + ion is oppositely directed to the magnetizing field. It is suggested that this anomaly is due to polarization of conduction electron spin associated with the doping Gd3 + ions.

  18. Neutron single crystal diffraction studies of orientational glass state in the [Rbx(NH4)1-x]3H(SO4)2 mixed crystals

    International Nuclear Information System (INIS)

    Smirnov, L.S.; Reehuis, M.; Loose, A.; Hohlwein, D.; Hoffmann, J.U.; Wozniak, K.; Dominiak, P.; Baranov, A.I.; Dolbinina, V.V.

    2005-01-01

    The [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystal with the concentration x=0.0 at room temperature crystallizes in a monoclinic C2/c with sp.gr. (space group), which is stabilized for x>0.09 down to low temperatures. This system is transformed in the orientational glass state below the freezing temperature T g =30 K. The differential Fourier maps for the [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals show that if for x=0.0 and 0.11 at 293 K the obtained maps reflect different orientational positions of crystallographically independent NH 4 (1) and NH 4 (2) groups, then the differential Fourier maps for x=0.20 at 9 K in the orientational glass state are similar for both ammonium groups reflecting their static disorder. The existence of the modulated structure in the [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals with x=0.11 at 2 K is discovered, while the modulated structure for x=0.20 at 2 K is absent. This observation supposes that there should be two different regions of the orientational glass state on x-T phase diagram of the [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals

  19. Solving crystal structures from neutron diffraction data

    International Nuclear Information System (INIS)

    Wilson, C.C.

    1987-07-01

    In order to pursue crystal structure determination using neutron diffraction data, and given the wide experience available of solving structures using X-ray data, the codes used in X-ray structural analysis should be adapted to the different requirements of a neutron experiment. Modifications have been made to a direct methods program MITHRIL and to a Patterson methods program PATMET to incorporate into these the features of neutron rather than X-ray diffraction. While to date these modifications have been fairly straightforward and many sophistications remain to be exploited, results obtained from the neutron versions of both programs are promising. (author)

  20. A theoretical overview on single hard diffraction

    International Nuclear Information System (INIS)

    Wuesthoff, M.

    1996-01-01

    The concept of the Pomeron structure function and its application in Single Hard Diffraction at hadron colliders and in diffractive Deep Inelastic Scattering is critically reviewed. Some alternative approaches are briefly surveyed with a focus on QCD inspired models

  1. Antiferromagnetism in chromium alloy single crystals

    DEFF Research Database (Denmark)

    Bjerrum Møller, Hans; Trego, A.L.; Mackintosh, A.R.

    1965-01-01

    The antiferromagnetism of single crystals of dilute alloys of V, Mn and Re in Cr has been studied at 95°K and 300°K by neutron diffraction. The addition of V causes the diffraction peaks to decrease in intensity and move away from (100), while Mn and Re cause them to increase and approach (100) s...

  2. High-pressure behavior of synthetic mordenite-Na. An in situ single-crystal synchrotron X-ray diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Lotti, Paolo; Merlini, Marco [Univ. degli Studi di Milano, (Italy). Dipt. di Scienze della Terra; Gatta, G. Diego [Univ. degli Studi di Milano, (Italy). Dipt. di Scienze della Terra; CNR, Bari (Italy). Int. di Cristallografia; Liermann, Hanns-Peter [DESY, Hamburg (Germany). Photon Sciences

    2015-05-01

    The high-pressure behavior of a synthetic mordenite-Na (space group: Cmcm or Cmc2{sub 1}) was studied by in situ single-crystal synchrotron X-ray diffraction with a diamond anvil cell up to 9.22(7) GPa. A phase transition, likely displacive in character, occurred between 1.68(7) and 2.70(8) GPa, from a C-centered to a primitive space group: possibly Pbnm, Pbnn or Pbn2{sub 1}. Fitting of the experimental data with III-BM equations of state allowed to describe the elastic behavior of the high-pressure polymorph with a primitive lattice. A very high volume compressibility [K{sub V0} = 25(2) GPa, β{sub V0} = 1/K{sub V0} = 0.040(3) GPa{sup -1}; K{sub V}' = (∂K{sub V}/∂P){sub T} = 2.0(3)], coupled with a remarkable elastic anisotropy (β{sub b}>>β{sub c}>β{sub a}), was found. Interestingly, the low-P and high-P polymorphs show the same anisotropic compressional scheme. A structure collapse was not observed up to 9.22(7) GPa, even though a strong decrease of the number of observed reflections at the highest pressures suggests an impending amorphization. The structure refinements performed at room-P, 0.98(2) and 1.68(7) GPa allowed to describe, at a first approximation, the mechanisms that govern the framework deformation in the low-P regime: the bulk compression is strongly accommodated by the increase of the ellipticity of the large 12-membered ring channels running along [001].

  3. Characterization of an Yb:LuVO{sub 4} single crystal using X-ray topography, high-resolution X-ray diffraction, and X-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Paszkowicz, W., E-mail: paszk@ifpan.edu.pl [Institute of Physics, Polish Academy of Sciences, al. Lotnikow 32/46, PL-02668 Warsaw (Poland); Romanowski, P.; Bak-Misiuk, J. [Institute of Physics, Polish Academy of Sciences, al. Lotnikow 32/46, PL-02668 Warsaw (Poland); Wierzchowski, W. [Institute of Electronic Materials Technology, Wolczynska 133, PL-01919 Warsaw (Poland); Wieteska, K. [Institute of Atomic Energy POLATOM, PL-05400 Otwock-Swierk (Poland); Graeff, W. [HASYLAB at DESY, Notkestr. 85, D-22603 Hamburg (Germany); Iwanowski, R.J. [Institute of Physics, Polish Academy of Sciences, al. Lotnikow 32/46, PL-02668 Warsaw (Poland); Heinonen, M.H. [Laboratory of Materials Science, Department of Physics, University of Turku, Vesilinnantie 5, FI-20014, Turku (Finland); Ermakova, O. [Institute of Physics, Polish Academy of Sciences, al. Lotnikow 32/46, PL-02668 Warsaw (Poland); Dabkowska, H. [Department of Physics, McMaster University, Hamilton, Ontario, L8S 4M1 (Canada)

    2011-10-15

    Knowledge on the defect and electronic structure allows for improved modeling of material properties. A short literature review has shown that the information on defect structure of rare earth orthovanadate single crystals is limited. In this paper, defect and electronic structure of a needle-shaped Yb:LuVO{sub 4} single crystal grown by the slow cooling method have been studied by means of X-ray diffraction topography employing white synchrotron beam, high-resolution diffraction (HRD) and photoelectron spectroscopy (XPS) techniques. Topographic investigations show that the crystal is composed of two blocks disoriented by about 1.5{sup o} and separated by a narrow deformed region. Some contrasts observed within the crystal volume may be attributed to glide bands and sector boundaries. The contrasts appearing in the vicinity of the surface may be interpreted as due to the presence of small inclusions. The HRD study indicates, in particular, that among point defects, the vacancy type defects dominate and that the density of other defects is small in comparison. The XPS measurements enabled, despite highly insulating properties of the studied crystal, an analysis of its bulk electronic structure, including the main core-levels (O 1s, V 2p, Lu 4f) as well as the valence band range.

  4. Direct observation of crystal texture by neutron diffraction topography

    International Nuclear Information System (INIS)

    Tomimitsu, Hiroshi

    1982-02-01

    This document reports the development and the applications of the neutron diffraction topography (NDT), which have been carried out at JAERI in these 10 years. This describes how the substructure of Cu-5%Ge single crystal of large-scale (3 cm in diameter and 10 cm in length) was revealed by the NDT-observation. It was discovered that the specimen crystal was made up from the layer-substructures parallel to (001) and to the [110] growth direction, and that each (001) layer-substructure mentioned above was further subdivided into the central thin sublayer parallel to (001) and thick plates of [100] and [010] directions, attached symmetrically to both sides of the central (001) sublayer with regular intervals. The model of the substructure described above was supported by the calculation of the diffraction intensities. The model of the layer-substructure described above, on the other hand, suggested a simple mechanism of crystal growth of the specimen. This document also reports the NDT-observation of the three-dimensional distribution of the lattice strains within a hot-pressed Ge single crystal, and the equal thickness fringes and the coherent boundaries of a twinned Si crystal. The powerfulness and the reliability of the NDT-technique were thus demonstrated. (author)

  5. Powder diffraction from a continuous microjet of submicrometer protein crystals.

    Science.gov (United States)

    Shapiro, D A; Chapman, H N; Deponte, D; Doak, R B; Fromme, P; Hembree, G; Hunter, M; Marchesini, S; Schmidt, K; Spence, J; Starodub, D; Weierstall, U

    2008-11-01

    Atomic-resolution structures from small proteins have recently been determined from high-quality powder diffraction patterns using a combination of stereochemical restraints and Rietveld refinement [Von Dreele (2007), J. Appl. Cryst. 40, 133-143; Margiolaki et al. (2007), J. Am. Chem. Soc. 129, 11865-11871]. While powder diffraction data have been obtained from batch samples of small crystal-suspensions, which are exposed to X-rays for long periods of time and undergo significant radiation damage, the proof-of-concept that protein powder diffraction data from nanocrystals of a membrane protein can be obtained using a continuous microjet is shown. This flow-focusing aerojet has been developed to deliver a solution of hydrated protein nanocrystals to an X-ray beam for diffraction analysis. This method requires neither the crushing of larger polycrystalline samples nor any techniques to avoid radiation damage such as cryocooling. Apparatus to record protein powder diffraction in this manner has been commissioned, and in this paper the first powder diffraction patterns from a membrane protein, photosystem I, with crystallite sizes of less than 500 nm are presented. These preliminary patterns show the lowest-order reflections, which agree quantitatively with theoretical calculations of the powder profile. The results also serve to test our aerojet injector system, with future application to femtosecond diffraction in free-electron X-ray laser schemes, and for serial crystallography using a single-file beam of aligned hydrated molecules.

  6. Polymorphous transformation in the crystal structure of [Mg(H.sub.2./sub.O).sub.6./sub. Br.sub.2./sub.][(C.sub.7./sub.H.sub.14./sub.N.sub.4./sub.).sub.2./sub.] . 4 (H.sub.2./sub.O) studied by powder and single crystal X-ray diffraction

    Czech Academy of Sciences Publication Activity Database

    Rivera, A.; Rohlíček, Jan; Sadat-Bernal, J.; Ríos-Motta, J.; Dušek, Michal

    2014-01-01

    Roč. 229, č. 4 (2014), s. 319-327 ISSN 0044-2968 Grant - others:AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : polymorphism * powder X-ray * single crystal diffraction * 1,3,6,8-tetraazatricyclo[4.3.1.13,ˑ 8]undecane * phase transformation * crystal structure analysis Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.310, year: 2014

  7. Single-crystal X-ray diffraction study of Cs2Er[Si6O14]F and Cs2Er[Si4O10]F

    International Nuclear Information System (INIS)

    Dabic, Predrag; Kremenovic, Aleksandar; Vulic, Predag; Kahlenberg, Volker; Schmidmair, Daniela

    2016-01-01

    Single-crystal growth experiments in the system CsF-Er 2 O 3 -SiO 2 resulted in the simultaneous crystallization of two chemically related compounds within the same run: Cs 2 Er[Si 6 O 14 ]F (phase I) and Cs 2 Er[Si 4 O 10 ]F (phase II). They represent the first examples for cesium erbium silicates containing fluorine. Basic crystallographic data are - phase I: space group Cmca, a=17.2556(6) Aa, b=24.6565(7) Aa, c=14.4735(5) Aa, V=6157.9(3) Aa 3 , Z=16; phase II: space group Pnma, a=22.3748(7) Aa, b=8.8390(2) Aa, c=11.9710(4) Aa, V=2367.5(1) Aa 3 , Z=8. The structures were determined by direct methods and refined to residuals of R(vertical stroke F vertical stroke)=0.0229 for 2920 (phase I) and 0.0231 for 2314 (phase II) independent observed reflections with I>2σ(I). The structure of phase I represents a previously unknown structure type with a three dimensional tetrahedral framework consisting of Q 3 and Q 4 groups in the ratio 2:1. Basic building units of the network are unbranched sechser single-chains running parallel to [001]. The network can be conveniently built up from the condensation of tetrahedral layers parallel to (010) or (100), respectively. The crystal structure of phase II can be classified as a tubular or columnar chain silicate indicating that the backbones of the structure are multiple chains of silicate tetrahedra. This structure is isotypic to a Cs 2 Y[Si 4 O 10 ]F, a compound that has been characterized previously. Alternatively, both compounds can be described as mixed octahedral-tetrahedral frameworks, which can be classified according to their polyhedral microensembles. A topological analysis of both nets is presented.

  8. Crystal diffraction lens telescope for focusing nuclear gamma rays

    International Nuclear Information System (INIS)

    Smither, R.K.; Fernandez, P.B.; Graber, T.; Faiz, M.

    1996-08-01

    A crystal diffraction lens was constructed at Argonne National Laboratory for use as a telescope to focus nuclear gamma rays. It consisted of 600 single crystals of germanium arranged in 8 concentric rings. The mounted angle of each crystal was adjusted to intercept and diffract the incoming gamma rays with an accuracy of a few arc sec. The performance of the lens was tested in two ways. In one case, the gamma rays were focused on a single medium size germanium detector. In the second case, the gamma rays were focused on the central germanium detector of a 3 x 3 matrix of small germanium detectors. The efficiency, image concentration and image quality, and shape were measured. The tests performed with the 3 x 3 matrix detector system were particularly interesting. The wanted radiation was concentrated in the central detector. The 8 other detectors were used to detect the Compton scattered radiation, and their energy was summed with coincident events in the central detector. This resulted in a detector with the efficiency of a large detector (all 9 elements) and the background of a small detector (only the central element). The use of the 3 x 3 detector matrix makes it possible to tell if the source is off axis and, if so, to tell in which direction. The crystal lens acts very much like a simple convex lens for visible light. Thus if the source is off to the left then the image will focus off to the right illuminating the detector on the right side: telling one in which direction to point the telescope. Possible applications of this type of crystal lens to balloon and satellite experiments will be discussed

  9. Diffraction and signal processing experiments with a liquid crystal microdisplay

    International Nuclear Information System (INIS)

    MartInez, Jose Luis; Moreno, Ignacio; Ahouzi, Esmail

    2006-01-01

    In this work, we show some diffraction experiments performed with a liquid crystal display (LCD) that shows how useful this device can be to teach and experience diffraction optics and signal processing experiments. The LCD acts as a programmable pixelated diffractive mask. The Fourier spectrum of the image displayed in the LCD is visualized through a simple free propagation diffraction experiment. This optical system allows easy testing of different diffractive elements. As a demonstration we include experimental results with well-known diffractive elements like diffraction gratings or Fresnel lenses, and with more complicated elements like computer-generated holograms

  10. Diffraction and signal processing experiments with a liquid crystal microdisplay

    Energy Technology Data Exchange (ETDEWEB)

    MartInez, Jose Luis [Departamento de Ciencia y TecnologIa de Materiales, Universidad Miguel Hernandez de Elche, Alicante (Spain); Moreno, Ignacio [Departamento de Ciencia y TecnologIa de Materiales, Universidad Miguel Hernandez de Elche, Alicante (Spain); Ahouzi, Esmail [Institut National des Postes et Telecomunications (INTP), Madinat Al Irfane, Rabat (Morocco)

    2006-09-01

    In this work, we show some diffraction experiments performed with a liquid crystal display (LCD) that shows how useful this device can be to teach and experience diffraction optics and signal processing experiments. The LCD acts as a programmable pixelated diffractive mask. The Fourier spectrum of the image displayed in the LCD is visualized through a simple free propagation diffraction experiment. This optical system allows easy testing of different diffractive elements. As a demonstration we include experimental results with well-known diffractive elements like diffraction gratings or Fresnel lenses, and with more complicated elements like computer-generated holograms.

  11. Dynamical neutron diffraction by curved crystals in the Laue geometry

    International Nuclear Information System (INIS)

    Albertini, G.; Melone, S.; Lagomarsino, S.; Mazkedian, S.; Puliti, P.; Rustichelli, F.

    1977-01-01

    The Taupin dynamical theory of X-ray diffraction by deformed crystals which was previously extended to the neutron diffraction by curved crystals in the Bragg geometry, is applied to calculate neutron diffraction patterns in the Laue geometry. The theoretical results are compared with experimental data on curved silicon crystals. The agreement is quite satisfactory. In the second part a simple model recently presented to describe neutron diffraction properties in the Bragg case is extended to the Laue case. The predictions of such a model are in satisfactory agreement with the rigorous theory and the experimental results. (author)

  12. Maximizing Macromolecule Crystal Size for Neutron Diffraction Experiments

    Science.gov (United States)

    Judge, R. A.; Kephart, R.; Leardi, R.; Myles, D. A.; Snell, E. H.; vanderWoerd, M.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    A challenge in neutron diffraction experiments is growing large (greater than 1 cu mm) macromolecule crystals. In taking up this challenge we have used statistical experiment design techniques to quickly identify crystallization conditions under which the largest crystals grow. These techniques provide the maximum information for minimal experimental effort, allowing optimal screening of crystallization variables in a simple experimental matrix, using the minimum amount of sample. Analysis of the results quickly tells the investigator what conditions are the most important for the crystallization. These can then be used to maximize the crystallization results in terms of reducing crystal numbers and providing large crystals of suitable habit. We have used these techniques to grow large crystals of Glucose isomerase. Glucose isomerase is an industrial enzyme used extensively in the food industry for the conversion of glucose to fructose. The aim of this study is the elucidation of the enzymatic mechanism at the molecular level. The accurate determination of hydrogen positions, which is critical for this, is a requirement that neutron diffraction is uniquely suited for. Preliminary neutron diffraction experiments with these crystals conducted at the Institute Laue-Langevin (Grenoble, France) reveal diffraction to beyond 2.5 angstrom. Macromolecular crystal growth is a process involving many parameters, and statistical experimental design is naturally suited to this field. These techniques are sample independent and provide an experimental strategy to maximize crystal volume and habit for neutron diffraction studies.

  13. Evidence for monoclinic distortion in the ground state phase of underdoped La_1_._9_5Sr_0_._0_5CuO_4: A single crystal neutron diffraction study

    International Nuclear Information System (INIS)

    Singh, Anar; Schefer, Jürg; Frontzek, Matthias; Sura, Ravi; Conder, Kazimierz; Sibille, Romain F.; Ceretti, Monica; Paulus, Werner

    2016-01-01

    The existing controversy about the symmetry of the crystal structure of the ground state of the critical doped La_1_._9_5Sr_0_._0_5CuO_4 has been resolved by analyzing the single crystal neutron diffraction data collected between 5 and 730 K. We observed small but significant intensities for “forbidden” reflections given by extinction rules of the orthorhombic Bmab space group at low temperatures. A careful investigation of neutron diffraction data reveals that the crystal structure of La_1_._9_5Sr_0_._0_5CuO_4 at 5 K is monoclinic with B2/m (2/m 1 1) space group. The monoclinic structure emerges from the orthorhombic structure in a continuous way; however, the structure is stable below ∼120 K which agrees with other observed phenomena. Our results on symmetry changes are crucial for the interpretation of physical properties also in other high temperature superconductors with similar structures.

  14. Ionothermal synthesis of β-NH4AlF4 and the determination by single crystal X-ray diffraction of its room temperature and low temperature phases

    International Nuclear Information System (INIS)

    Parnham, Emily R.; Slawin, Alex M.Z.; Morris, Russell E.

    2007-01-01

    β-NH 4 AlF 4 has been synthesised ionothermally using 1-ethyl-3-methylimidazolium hexafluorophosphate as solvent and template provider. β-NH 4 AlF 4 crystals were produced which were suitable for single crystal X-ray diffraction analysis. A phase transition occurs between room temperature (298 K) and low temperature (93 K) data collections. At 298 K the space group=I4/mcm (no. 140), α=11.642(5), c=12.661(5) A, Z=2 (10NH 4 AlF 4 ), wR(F 2 )=0.1278, R(F)=0.0453. At 93 K the space group=P4 2 /ncm (no. 138), α=11.616(3), c=12.677(3) A, Z=2 (10NH 4 AlF 4 ), wR(F 2 )=0.1387, R(F)=0.0443. The single crystal X-ray diffraction study of β-NH 4 AlF 4 shows the presence of two different polymorphs at low and room temperature, indicative of a phase transition. The [AlF 4/2 F 2 ] - layers are undisturbed except for a small tilting of the AlF 6 octahedra in the c-axis direction. -Ionothermal synthesis, the use of an ionic liquid as the solvent in materials preparation, has been used to prepare β-NH 4 AlF 4 , and structural characterisation indicates that there are two versions of the structure, a low temperature primitive phase at 93 K and a high temperature body-centered phase at 298 K

  15. Structures of plutonium coordination compounds: A review of past work, recent single crystal x-ray diffraction results, and what we're learning about plutonium coordination chemistry

    Science.gov (United States)

    Neu, M. P.; Matonic, J. H.; Smith, D. M.; Scott, B. L.

    2000-07-01

    The compounds we have isolated and characterized include plutonium(III) and plutonium(IV) bound by ligands with a range of donor types and denticity (halide, phosphine oxide, hydroxamate, amine, sulfide) in a variety of coordination geometries. For example, we have obtained the first X-ray structure of Pu(III) complexed by a soft donor ligand. Using a "one pot" synthesis beginning with Pu metal strips and iodine in acetonitrile and adding trithiacyclononane we isolated the complex, PuI3(9S3)(MeCN)2 (Figure 1). On the other end of the coordination chemistry spectrum, we have obtained the first single crystal structure of the Pu(IV) hexachloro anion (Figure 2). Although this species has been used in plutonium purification via anion exchange chromatography for decades, the bond distances and exact structure were not known. We have also characterized the first plutonium-biomolecule complex, Pu(IV) bound by the siderophore desferrioxamine E.In this presentation we will review the preparation, structures, and importance of previously known coordination compounds and of those we have recently isolated. We will show the coordination chemistry of plutonium is rich and varied, well worth additional exploration.

  16. Friction stir welding of single crystal aluminium

    DEFF Research Database (Denmark)

    Fonda, Richard Warren; Wert, John A.; Reynolds, A.P.

    2007-01-01

    Friction stir welds were prepared in different orientations in an aluminium single crystal. The welds were quenched to preserve the microstructure surrounding the tool and then electron backscattered diffraction was used to reveal the generation of grain boundaries and the evolution...... of crystallographic texture around the tool in each weld. The extent of both dynamic recrystallisation and conventional recrystallisation varied considerably as a function of weld orientation. As the base plate begins to interact with the deformation field surrounding the tool, regions of the single crystal rotate...

  17. Symmetry, stability, and diffraction properties of icosahedral crystals

    International Nuclear Information System (INIS)

    Bak, P.

    1985-01-01

    In a remarkable experiment on an Mn-Al alloy, Shechtman et al. observed a diffraction spectrum with icosahedral symmetry. This is inconsistent with discrete translational invariance since the symmetry includes a five-fold axis. In this paper, it is shown that the crystallography and diffraction pattern can be described by a six-dimensional space group. The crystal structure in 3d is obtained as a cut along a 3d hyperplane in a regular 6d crystal. Displacements of the 6d crystal along 6 orthogonal directions define 6 continuous symmetries for the icosahedral crystal, three of which are phase symmetries describing internal rearrangements of the atoms

  18. Crystal structure of aspartame anhydrate from powder diffraction data. Structural aspects of the dehydration process of aspartame

    NARCIS (Netherlands)

    Guguta, C.; Meekes, H.L.M.; Gelder, R. de

    2006-01-01

    Aspartame has three pseudo-polymorphic forms, two hydrates and a hemi-hydrate, for which crystal structures were determined from single-crystal diffraction data. This paper presents the crystal structure of the anhydrate, which was obtained by dehydrating the hemi-hydrate. The crystal structure of

  19. Effect of cationic substitution on the double-well hydrogen-bond potential in [K1-x(NH4)x]3H(SO4)2 proton conductors: a single-crystal neutron diffraction study.

    Science.gov (United States)

    Choudhury, R R; Chitra, R; Selezneva, E V; Makarova, I P

    2017-10-01

    The structure of the mixed crystal [K 1-x (NH 4 ) x ] 3 H(SO 4 ) 2 as obtained from single-crystal neutron diffraction is compared with the previously reported room-temperature neutron structure of crystalline K 3 H(SO 4 ) 2 . The two structures are very similar, as indicated by the high value of their isostructurality index (94.8%). It was found that the replacement of even a small amount (3%) of K + with NH 4 + has a significant influence on the short strong hydrogen bond connecting the two SO 4 2- ions. Earlier optical measurements had revealed that the kinetics of the superionic transition in the solid solution [K 1-x (NH 4 ) x ] 3 H(SO 4 ) 2 are much faster than in K 3 H(SO 4 ) 2 ; this reported difference in the kinetics of the superionic phase transition in this class of crystal is explained on the basis of the difference in strength of the hydrogen-bond interactions in the two structures.

  20. Polarity of wurtzite crystals by photoelectron diffraction

    Czech Academy of Sciences Publication Activity Database

    Bartoš, Igor; Romanyuk, Olexandr

    2014-01-01

    Roč. 315, OCT (2014), s. 506-509 ISSN 0169-4332 Grant - others:AVČR(CZ) M100101201 Institutional support: RVO:68378271 Keywords : wurtzite semiconductors * surface polarity * X-ray photoelectron diffraction * XPD Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.711, year: 2014 http://www.sciencedirect.com/science/article/pii/S016943321400066X

  1. Solvent exchange in a metal–organic framework single crystal monitored by dynamic in situ X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cox, Jordan M.; Walton, Ian M.; Bateman, Gage; Benson, Cassidy A.; Mitchell, Travis; Sylvester, Eric; Chen, Yu-Sheng; Benedict, Jason B. (UC); (Buffalo)

    2017-07-25

    Understanding the processes by which porous solid-state materials adsorb and release guest molecules would represent a significant step towards developing rational design principles for functional porous materials. To elucidate the process of liquid exchange in these materials, dynamicin situX-ray diffraction techniques have been developed which utilize liquid-phase chemical stimuli. Using these time-resolved diffraction techniques, the ethanol solvation process in a flexible metal–organic framework [Co(AIP)(bpy)0.5(H2O)]·2H2O was examined. The measurements provide important insight into the nature of the chemical transformation in this system including the presence of a previously unreported neat ethanol solvate structure.

  2. Crystal structure redetermination of ε-Ni.sub.3./sub.Si.sub.2./sub. from a single nanowire by dynamical refinement of precession electron diffraction data

    Czech Academy of Sciences Publication Activity Database

    Correa, Cinthia Antunes; Klementová, Mariana; Dřínek, Vladislav; Kopeček, Jaromír; Palatinus, Lukáš

    2016-01-01

    Roč. 672, Jul (2016), s. 505-509 ISSN 0925-8388 R&D Projects: GA ČR GA13-25747S Institutional support: RVO:68378271 ; RVO:67985858 Keywords : precession electron diffraction tomography * structure determination * nanowire * dynamical refinement Subject RIV: BM - Solid Matter Physics ; Magnetism; CA - Inorganic Chemistry (UCHP-M) OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.); Inorganic and nuclear chemistry (UCHP-M) Impact factor: 3.133, year: 2016

  3. Structure and microstructure of Ni-Mn-Ga single crystal exhibiting magnetic shape memory effect analysed by high resolution X-ray diffraction

    Czech Academy of Sciences Publication Activity Database

    Heczko, Oleg; Cejpek, P.; Drahokoupil, Jan; Holý, V.

    2016-01-01

    Roč. 115, Aug (2016), s. 250-258 ISSN 1359-6454 R&D Projects: GA ČR GA13-30397S; GA ČR GA15-00262S Institutional support: RVO:68378271 Keywords : magnetic field-induced strain * magnetic shape memory effect * X-ray diffraction * structure of Ni-Mn-Ga Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 5.301, year: 2016

  4. Single-Crystal X-Ray Diffraction Studies of Homologues in the Series nBa(Nb,Zr)O 3+3 mNbO with n=2, 3, 4, 5 and m=1

    Science.gov (United States)

    Nilsson, G.; Svensson, G.

    2001-01-01

    Single crystals of four homologues in the series nBa(Nb,Zr)O3+3mNbO, with n:m=2:1, 3:1, 4:1, and 5:1, were found in the reduced Ba-Nb-Zr-O system. Single-crystal X-ray diffraction data were collected for all the crystals. For all homologues the space group was found to be P4/mmm. The structures can be described as intergrowths of Ba(Nb,Zr)O3 perovskite and NbO slabs. The refined cell parameters and compositions of the 2:1, 3:1, and 4:1 homologues are a=4.1768(5) Å and c=12.269(2) Å for Ba2Nb4.5(1)Zr0.5(1)O9, a=4.1769(5) Å and c=16.493(3) Å for Ba3+δNb4.8(2)-δ Zr1.2(2)O12-δ (δ=0.098(4)), and a=4.1747(6) Å and c= 20.619(4) Å for Ba4+δNb5.1(4)-δZr1.9(4)O15-δ (δ=0.270(9)). The refined cell parameters of the 5:1 homologue are a=4.1727(3) Å and c=24.804(3) Å. Zr replaces Nb only in the NbO6 octahedra found in the perovskite slabs.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  6. Neutron magnetic multiple diffraction in a natural magnetite crystal

    International Nuclear Information System (INIS)

    Mazzocchi, V.L.; Parente, C.B.R.

    1988-09-01

    Neutron multiple diffraction has been employed in the study of the magnetism in magnetite (Fe 3 O 4 ). Magnetite has a crystallographic structure of an inverted spinel with tetrahedral A sites occupied solely by trivalent Fe 3+ ions and octahedral B sites occupied both by divalent Fe 2+ ions and the remaining Fe 3+ ions in random distribution. At room temperature magnetite is a Neel A-B ferrimagnet where the ions on the A, B sites are coupled antiferromagneticaly. This coupling disappears at T sup c approx. or approx.= 580 0 C. Employing a natural single crystal of magnetite experimental neutron multiple diffraction patterns were obtained for the primary reflection 111 at room temperature and 703 0 C. This reflection is almost entirely magnetic in origin resulting in 'Aufhellung' patterns below T c and mixed 'Aufhellung-Umweganregung' patterns above T c . Theoretical patterns were calculated employing the iterative method for the approximation of intensities by a Taylor series and compared to the experimental results. (author) [pt

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  8. Single Crystal Diffractometry

    Science.gov (United States)

    Arndt, U. W.; Willis, B. T. M.

    2009-06-01

    Preface; Acknowledgements; Part I. Introduction; Part II. Diffraction Geometry; Part III. The Design of Diffractometers; Part IV. Detectors; Part V. Electronic Circuits; Part VI. The Production of the Primary Beam (X-rays); Part VII. The Production of the Primary Beam (Neutrons); Part VIII. The Background; Part IX. Systematic Errors in Measuring Relative Integrated Intensities; Part X. Procedure for Measuring Integrated Intensities; Part XI. Derivation and Accuracy of Structure Factors; Part XII. Computer Programs and On-line Control; Appendix; References; Index.

  9. Time-resolved Laue diffraction from protein crystals: Instrumental considerations

    International Nuclear Information System (INIS)

    Bilderback, D.H.; Cornell Univ., Ithaca, NY; Moffat, K.; Szebenyi, D.M.E.

    1984-01-01

    A serious limitation of macromolecular crystallography has been its inability to determine changes in structure on a biochemical time scale of milliseconds or less. Recently, we have shown that X-ray exposures on single crystals of macromolecules may be obtained in the millisecond time range through the use of intense, polychromatic radiation with Δlambda/lambda approx.= 0.2 derived from the Cornell High Energy Synchrotron Source, CHESS. Such radiation falling on a stationary crystal yields a Laue diffraction pattern, in which almost all Laue reflections arise from a unique set of Miller indices and where their intensities are automatically integrated over wavelength. This Laue technique requires wide band pass optics, which may be obtained by a combination of reflection and transmission mirrors, filters or layered synthetic microstructures. Time-resolved macromolecular crystallography may be achieved by several data collection schemes: 'one-shot' recording coupled to a simple streak camera, repetitive sample perturbation coupled to a detector with temporal resolution and repetitive perturbation which uses the synchrotron pulses for stroboscopic triggering and detection. These schemes are appropriate for different time scales, roughly the milli-, micro- and nanosecond regimes. It appears that time-resolved crystallography is entirely feasible, with an ultimate time resolution limited only by the length of a synchrotron light pulse, some 150 ps at CHESS. (orig.)

  10. Intergrown new zeolite beta polymorphs with interconnected 12-ring channels solved by combining electron crystallography and single-crystal X-ray diffraction

    KAUST Repository

    Yu, Zhengbao; Han, Yu; Zhao, Lan; Huang, Shiliang; Zheng, Qiyu; Lin, Shuangzheng; Cõ rdova, Armando C.; Zou, Xiaodong; Sun, Junliang

    2012-01-01

    Two new polymorphs of zeolite beta, denoted as SU-78A and SU-78B, were synthesized by employing dicyclohexylammonium hydroxides as organic structure-directing agents. The structure was solved by combining transmission electron microscopy and single

  11. Crystallization and diffraction analysis of thioredoxin reductase from Streptomyces coelicolor

    International Nuclear Information System (INIS)

    Koháryová, Michaela; Brynda, Jiří; Řezáčová, Pavlína; Kollárová, Marta

    2011-01-01

    Thioredoxin reductase from S. coelicolor was crystallized and diffraction data were collected to 2.4 Å resolution. Thioredoxin reductases are homodimeric flavoenzymes that catalyze the transfer of electrons from NADPH to oxidized thioredoxin substrate. Bacterial thioredoxin reductases represent a promising target for the development of new antibiotics. Recombinant thioredoxin reductase TrxB from Streptomyces coelicolor was crystallized using the hanging-drop vapour-diffusion method. X-ray diffraction data were collected from cryocooled crystals to 2.4 Å resolution using a synchrotron-radiation source. The crystals belonged to the primitive monoclinic space group P2 1 , with unit-cell parameters a = 82.9, b = 60.6, c = 135.4 Å, α = γ = 90.0, β = 96.5°

  12. A multistep single-crystal-to-single-crystal bromodiacetylene dimerization

    Science.gov (United States)

    Hoheisel, Tobias N.; Schrettl, Stephen; Marty, Roman; Todorova, Tanya K.; Corminboeuf, Clémence; Sienkiewicz, Andrzej; Scopelliti, Rosario; Schweizer, W. Bernd; Frauenrath, Holger

    2013-04-01

    Packing constraints and precise placement of functional groups are the reason that organic molecules in the crystalline state often display unusual physical or chemical properties not observed in solution. Here we report a single-crystal-to-single-crystal dimerization of a bromodiacetylene that involves unusually large atom displacements as well as the cleavage and formation of several bonds. Density functional theory computations support a mechanism in which the dimerization is initiated by a [2 + 1] photocycloaddition favoured by the nature of carbon-carbon short contacts in the crystal structure. The reaction proceeded up to the theoretical degree of conversion without loss of crystallinity, and it was also performed on a preparative scale with good yield. Moreover, it represents the first synthetic pathway to (E)-1,2-dibromo-1,2-diethynylethenes, which could serve as synthetic intermediates for the preparation of molecular carbon scaffolds. Our findings both extend the scope of single-crystal-to-single-crystal reactions and highlight their potential as a synthetic tool for complex transformations.

  13. Surface quality inspection of PbWO4 crystals by grazing incidence X-ray diffraction

    International Nuclear Information System (INIS)

    Mengucci, P.; Di Cristoforo, A.; Lebeau, M.; Majni, G.; Paone, N.; Pietroni, P.; Rinaldi, D.

    2005-01-01

    High-quality scintillating crystals are required for applications in radiographic systems and high-energy physics detectors to achieve the specified optical properties. In order to study the state of the single crystals surface we propose the use of the grazing incidence X-ray diffraction (GID) technique. This technique allows performing a depth profiling of the sample by changing the incidence angle of the X-ray beam with respect to the sample surface. In this work, two samples of a large PbWO 4 (PWO) single crystal exhibiting different surface roughness values have been studied. Results have shown that GID is a suitable technique for surface quality inspection

  14. Properties of single crystal beta''-aluminas

    International Nuclear Information System (INIS)

    Bates, J.B.; Brown, G.M.; Kaneda, T.; Brundage, W.E.; Wang, J.C.; Engstrom, H.

    1979-01-01

    Large single crystals of sodium beta''-alumina were grown by slow evaporation of Na 2 O at 1690 0 C from a mixture of Na 2 CO 3 , MgO, and Al 2 O 3 . Polarized Raman measurements were made on the Na β'' single crystals and on single crystals of Li, K, Rb, and Ag β'' prepared by ion exchange of Na β''. The low frequency Raman spectra of Na, K, Rb, and Ag β'' contained four or more bands due to vibrations of the mobile cations. These results were analyzed by assuming the spectra to be due to the normal modes of a defect cluster consisting of a cation vacancy surrounded by three cations. From model calculations, the Raman band of Na β'' at 33 cm -1 is assigned to the attempt mode for diffusion of Na + ions. The structure of a Ag β'' single crystal was investigated by neutron diffraction, and 20% of the Ag + ion sites were found to be vacant

  15. Feasibility of one-shot-per-crystal structure determination using Laue diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cornaby, Sterling [School of Applied and Engineering Physics, Cornell University, Ithaca, New York (United States); CHESS (Cornell High Energy Synchrotron Source), Cornell University, Ithaca, New York (United States); Szebenyi, Doletha M. E. [MacCHESS (Macromolecular Diffraction Facilities at CHESS), Cornell University, Ithaca, New York (United States); Smilgies, Detlef-M. [CHESS (Cornell High Energy Synchrotron Source), Cornell University, Ithaca, New York (United States); Schuller, David J.; Gillilan, Richard; Hao, Quan [MacCHESS (Macromolecular Diffraction Facilities at CHESS), Cornell University, Ithaca, New York (United States); Bilderback, Donald H., E-mail: dhb2@cornell.edu [School of Applied and Engineering Physics, Cornell University, Ithaca, New York (United States); CHESS (Cornell High Energy Synchrotron Source), Cornell University, Ithaca, New York (United States)

    2010-01-01

    Structure determination was successfully carried out using single Laue exposures from a group of lysozyme crystals. The Laue method may be a viable option for collection of one-shot-per-crystal data from microcrystals. Crystal size is an important factor in determining the number of diffraction patterns which may be obtained from a protein crystal before severe radiation damage sets in. As crystal dimensions decrease this number is reduced, eventually falling to one, at which point a complete data set must be assembled using data from multiple crystals. When only a single exposure is to be collected from each crystal, the polychromatic Laue technique may be preferable to monochromatic methods owing to its simultaneous recording of a large number of fully recorded reflections per image. To assess the feasibility of solving structures using single Laue images from multiple crystals, data were collected using a ‘pink’ beam at the CHESS D1 station from groups of lysozyme crystals with dimensions of the order of 20–30 µm mounted on MicroMesh grids. Single-shot Laue data were used for structure determination by molecular replacement and correct solutions were obtained even when as few as five crystals were used.

  16. Feasibility of one-shot-per-crystal structure determination using Laue diffraction

    International Nuclear Information System (INIS)

    Cornaby, Sterling; Szebenyi, Doletha M. E.; Smilgies, Detlef-M.; Schuller, David J.; Gillilan, Richard; Hao, Quan; Bilderback, Donald H.

    2010-01-01

    Structure determination was successfully carried out using single Laue exposures from a group of lysozyme crystals. The Laue method may be a viable option for collection of one-shot-per-crystal data from microcrystals. Crystal size is an important factor in determining the number of diffraction patterns which may be obtained from a protein crystal before severe radiation damage sets in. As crystal dimensions decrease this number is reduced, eventually falling to one, at which point a complete data set must be assembled using data from multiple crystals. When only a single exposure is to be collected from each crystal, the polychromatic Laue technique may be preferable to monochromatic methods owing to its simultaneous recording of a large number of fully recorded reflections per image. To assess the feasibility of solving structures using single Laue images from multiple crystals, data were collected using a ‘pink’ beam at the CHESS D1 station from groups of lysozyme crystals with dimensions of the order of 20–30 µm mounted on MicroMesh grids. Single-shot Laue data were used for structure determination by molecular replacement and correct solutions were obtained even when as few as five crystals were used

  17. The new single crystal diffractometer SC3

    International Nuclear Information System (INIS)

    Schefer, J.; Koch, M.; Keller, P.; Fischer, S.; Thut, R.

    1996-01-01

    Single crystal diffraction is a powerful method for the determination of precise structure parameters, superlattices, stress. Neutron single crystal diffraction gives additionally to X-rays information on magnetic structures, both commensurate and incommensurate, hydrogen positions, hydrogen bonding behavior and accurate bondlengths, e.g. important in cuprates. The method is therefore especially powerful if combined with X-ray diffraction results. The new instrument at SINQ has been designed for inorganic materials and is positioned at a thermal beam tube, pointing on a water scatterer. This scatterer is presently operating with H 2 O at ambient temperature, but a change to another medium at different temperature is possible. The instrument will be equipped with three area detectors, moving at fixed difference in 2Θ. each detector may be individually moved around a vertical circle (tilting angle γ), allowing to use not only 4-circle geometry in the temperature range from 1.5 to 380 K, but also any equipment from a dilution refrigerator (7 mK) to a heavy magnet. A high temperature furnace for 4-circle geometry is foreseen as a future option. (author) 6 figs., 1 tab., 7 refs

  18. The new single crystal diffractometer SC3

    Energy Technology Data Exchange (ETDEWEB)

    Schefer, J; Koch, M; Keller, P; Fischer, S; Thut, R [Lab. for Neutron Scattering ETH Zurich, Zurich (Switzerland) and Paul Scherrer Institute, Villigen (Switzerland)

    1996-11-01

    Single crystal diffraction is a powerful method for the determination of precise structure parameters, superlattices, stress. Neutron single crystal diffraction gives additionally to X-rays information on magnetic structures, both commensurate and incommensurate, hydrogen positions, hydrogen bonding behavior and accurate bondlengths, e.g. important in cuprates. The method is therefore especially powerful if combined with X-ray diffraction results. The new instrument at SINQ has been designed for inorganic materials and is positioned at a thermal beam tube, pointing on a water scatterer. This scatterer is presently operating with H{sub 2}O at ambient temperature, but a change to another medium at different temperature is possible. The instrument will be equipped with three area detectors, moving at fixed difference in 2{Theta}. each detector may be individually moved around a vertical circle (tilting angle {gamma}), allowing to use not only 4-circle geometry in the temperature range from 1.5 to 380 K, but also any equipment from a dilution refrigerator (7 mK) to a heavy magnet. A high temperature furnace for 4-circle geometry is foreseen as a future option. (author) 6 figs., 1 tab., 7 refs.

  19. Phase modulation due to crystal diffraction by ptychographic imaging

    Science.gov (United States)

    Civita, M.; Diaz, A.; Bean, R. J.; Shabalin, A. G.; Gorobtsov, O. Yu.; Vartanyants, I. A.; Robinson, I. K.

    2018-03-01

    Solving the phase problem in x-ray crystallography has occupied a considerable scientific effort in the 20th century and led to great advances in structural science. Here we use x-ray ptychography to demonstrate an interference method which measures the phase of the beam transmitted through a crystal, relative to the incoming beam, when diffraction takes place. The observed phase change of the direct beam through a small gold crystal is found to agree with both a quasikinematical model and full dynamical theories of diffraction. Our discovery of a diffraction contrast mechanism will enhance the interpretation of data obtained from crystalline samples using the ptychography method, which provides some of the most accurate x-ray phase-contrast images.

  20. Single Crystal Surfaces

    Science.gov (United States)

    Aguilar-Santillan, Joaquin

    2014-06-01

    The present work studies (0001) Al2O3 and (111) Al2MgO4 wetting with pure molten Al by the sessile drop technique from 1073 K to 1473 K (800 °C to 1200 °C) under Ar at PO2 10-15 Pa. Al pure liquid wets a smooth and chemically homogeneous surface of an inert solid, the wetting driving force ( t, T) can be readily studied when surface solid roughness increases in the system. Both crystals planes (0001) Al2O3 and (111) Al2MgO4 have crystallographic surfaces with identical O-2 crystalline positions however considering Mg2+ content in Al2MgO4 structure may influence a reactive mode. Kinetic models results under similar experimental conditions show that Al wetting on (0001) Al2O3 is less reactive than (111) Al2MgO4, however at >1273 K (1000 °C) (0001) Al2O3 transformation occurs and a transition of wetting improves. The (111) Al2MgO4 and Al system promotes interface formations that slow its wetting process.

  1. Crystal structure of core streptavidin determined from multi-wavelength anomalous diffraction of synchrotron radiation

    International Nuclear Information System (INIS)

    Hendrickson, W.A.; Paehler, A.; Smith, J.L.; Satow, Y.; Merritt, E.A.; Phizackerley, R.P.

    1989-01-01

    A three-dimensional crystal structure of the biotin-binding core of streptavidin has been determined at 3.1-angstrom resolution. The structure was analyzed from diffraction data measured at three wavelengths from a single crystal of the selenobiotinyl complex with streptavidin. Streptavidin is a tetramer with subunits arrayed in D 2 symmetry. Each protomer is an 8-stranded β-barrel with simple up-down topology. Biotin molecules are bound at one end of each barrel. This study demonstrates the effectiveness of multi-wavelength anomalous diffraction (MAD) procedures for macromolecular crystallography and provides a basis for detailed study of biotin-avidin interactions

  2. Serial single molecule electron diffraction imaging: diffraction background of superfluid helium droplets

    Science.gov (United States)

    Zhang, Jie; He, Yunteng; Lei, Lei; Alghamdi, Maha; Oswalt, Andrew; Kong, Wei

    2017-08-01

    In an effort to solve the crystallization problem in crystallography, we have been engaged in developing a method termed "serial single molecule electron diffraction imaging" (SS-EDI). The unique features of SS-EDI are superfluid helium droplet cooling and field-induced orientation: together the two features constitute a molecular goniometer. Unfortunately, the helium atoms surrounding the sample molecule also contribute to a diffraction background. In this report, we analyze the properties of a superfluid helium droplet beam and its doping statistics, and demonstrate the feasibility of overcoming the background issue by using the velocity slip phenomenon of a pulsed droplet beam. Electron diffraction profiles and pair correlation functions of ferrocene-monomer-doped droplets and iodine-nanocluster-doped droplets are presented. The timing of the pulsed electron gun and the effective doping efficiency under different dopant pressures can both be controlled for size selection. This work clears any doubt of the effectiveness of superfluid helium droplets in SS-EDI, thereby advancing the effort in demonstrating the "proof-of-concept" one step further.

  3. Single-crystal growth of ceria-based materials

    International Nuclear Information System (INIS)

    Ulbrich, Gregor

    2015-01-01

    In this work it could be shown that Skull-Melting is a suitable method for growing ceria single crystals. Twenty different ceria-based single crystals could be manufactured. It was possible to dope ceria single crystals with Gd, Sm, Y, Zr, Ti, Ta, and Pr in different concentrations. Also co-doping with the named metals was realized. However, there remain some problems for growing ceria-based single crystals by Skull-Melting. As ignition metal zirconium was used because no ceria-based material works well. For that reason all single crystals show small zirconium contamination. Another problem is the formation of oxygen by the heat-induced reduction of ceria during the melting process. Because of that the skull of sintered material is often destroyed by gas pressure. This problem had to be solved individually for every single crystal. The obtained single crystals were characterized using different methods. To ensure the single crystal character the y were examined by Laue diffraction. All manufactured crystals are single crystals. Also powder diffraction patterns of the milled and oxidized samples were measured. For the determination of symmetry and metric the structural parameters were analyzed by the Rietveld method. All synthesized materials crystallize in space group Fm-3m known from calcium fluoride. The cubic lattice parameter a was determined for all crystals. In the case of series with different cerium and zirconium concentrations a linear correlation between cerium content and cubic lattice parameter was detected. The elemental composition was determined by WDX. All crystals show a homogeneous elemental distribution. The oxygen content was calculated because the WDX method isn't useful for determination.

  4. Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto.

    Science.gov (United States)

    Yanagisawa, Yasuhide; Chatake, Toshiyuki; Chiba-Kamoshida, Kaori; Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki; Yasuda, Ichiro; Morimoto, Yukio

    2010-12-01

    Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27,724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a=74.3, b=49.9, c=56.3 Å, β=95.2°. Diffraction images were processed to a resolution of 1.74 Å with an Rmerge of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase.

  5. Crystal ball single event display

    International Nuclear Information System (INIS)

    Grosnick, D.; Gibson, A.; Allgower, C.; Alyea, J.; Argonne National Lab., IL

    1997-01-01

    The Single Event Display (SED) is a routine that is designed to provide information graphically about a triggered event within the Crystal Ball. The SED is written entirely in FORTRAN and uses the CERN-based HICZ graphing package. The primary display shows the amount of energy deposited in each of the NaI crystals on a Mercator-like projection of the crystals. Ten different shades and colors correspond to varying amounts of energy deposited within a crystal. Information about energy clusters is displayed on the crystal map by outlining in red the thirteen (or twelve) crystals contained within a cluster and assigning each cluster a number. Additional information about energy clusters is provided in a series of boxes containing useful data about the energy distribution among the crystals within the cluster. Other information shown on the event display include the event trigger type and data about π o 's and η's formed from pairs of clusters as found by the analyzer. A description of the major features is given, along with some information on how to install the SED into the analyzer

  6. Influence of solvents on the habit modification of alpha lactose monohydrate single crystals

    Science.gov (United States)

    Parimaladevi, P.; Srinivasan, K.

    2013-02-01

    Restricted evaporation of solvent method was adopted for the growth of alpha lactose monohydrate single crystals from different solvents. The crystal habits of grown crystals were analysed. The form of crystallization was confirmed by powder x-ray diffraction analysis. Thermal behaviour of the grown crystals was studied by using differential scanning calorimetry.

  7. Neutron Diffraction Study of the Irreversible R-MA-MC Phase Transition in Single Crystal Pb[(Zn1/3Nb2/3)1-xTix]O3

    NARCIS (Netherlands)

    Ohwada, Kenji; Hirota, Kazuma; Rehrig, Paul W.; Gehring, Peter M.; Noheda, Beatriz; Fujii, Yasuhiko; Park, Seung-Eek Eagle; Shirane, Gen

    2001-01-01

    Single crystals of the relaxor PZN-xPT display an enormously strong piezoelectric character. Recent x-ray scattering studies have revealed novel electric-field induced phase transitions in PZN-8%PT. As-grown crystals exhibit a rhombohedral structure that, under application of an electric field

  8. Structure of single-chain single crystals of isotactic polystyrene and their radiation resistance

    International Nuclear Information System (INIS)

    Bu Haishan; Cao Jie; Xu Shengyong; Zhang Ze

    1997-01-01

    The structure of the single-chain single crystals of isotactic polystyrene (i-PS) was investigated by electron diffraction (ED) and high resolution electron microscopy (HREM). The nano-scale single-chain single crystals were found to be very stable to electron irradiation. According to the unit cell of i-PS crystals, the reflection rings in ED pattern and the lattice fringes in HREM images could be indexed, but the lower-index diffractions were not found. It is proposed that the single-chain single crystals are very small, thus secondary electrons may be allowed to escape and radiation damage is highly reduced, and that there are less lower-index lattice planes in the single-chain single crystals to provide sufficient diffraction intensity for recording. HREM images can be achieved at room temperature in the case of single-chain single crystals because of its stability to electron irradiation, therefore, this might be a novel experimental approach to the study of crystal structure of macromolecules

  9. Preliminary study of a phase transformation in insulin crystals using synchrotron-radiation Laue diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Reynolds, C D; Stowell, B; Joshi, K K; Harding, M M; Maginn, S J; Dodson, G G

    1988-10-01

    Synchrotron-radiation Laue diffraction photographs have been recorded showing the transformation of single 4Zn insulin crystals (a=80.7 (1), c=37.6 (1) A, space group R3) to 2Zn insulin (a=82.5 (1), c=34.0 (1) A, space group R3). The transformation was brought about by changing the mother liquor in the capillary in which the crystal was mounted. Photographs were taken at 10 min intervals (exposure time 3 s) from 0.5 h after mounting. They showed initially a well ordered 4Zn insulin crystal (d/sub min/ ca 2.3 A), then a poorly ordered, sometimes multiple, crystal, and finally a 2Zn insulin crystal, about as well ordered as the initial crystal.

  10. Habit modification of nearly perfect single crystals of potassium dihydrogen phosphate (KDP) by trivalent manganese ions studied using synchrotron radiation X-ray multiple diffraction in Renninger scanning mode

    OpenAIRE

    Lai, X; Roberts, KJ; Avanci, LH; Cardoso, LP; Sasaki, JM

    2003-01-01

    The X-ray multiple diffraction technique using synchrotron radiation is applied in the preliminary study of the habit modification of KDP samples as induced by incorporation of the trivalent transition metal cation Mn3+. High-resolution Renninger scans of pure and doped KDP were carried out using 400 as the primary reflection, echoing the fact that these impurity species were segregated in the {100} growth sector. The analysis of the Renninger scans of the doped KDP crystals is consistent wit...

  11. Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto

    International Nuclear Information System (INIS)

    Yanagisawa, Yasuhide; Chatake, Toshiyuki; Chiba-Kamoshida, Kaori; Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki; Yasuda, Ichiro; Morimoto, Yukio

    2010-01-01

    Nattokinase, a protein found in high levels in the traditional Japanese food natto, has been reported to have high thrombolytic activity. In the present study, the crystallization of native nattokinase and the collection of X-ray diffraction date from a nattokinase crystal to a resolution of 1.74 Å are reported. Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27 724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a = 74.3, b = 49.9, c = 56.3 Å, β = 95.2°. Diffraction images were processed to a resolution of 1.74 Å with an R merge of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase

  12. Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto

    Energy Technology Data Exchange (ETDEWEB)

    Yanagisawa, Yasuhide [Faculty of Pharmaceutical Sciences, Chiba Institute of Science, 15-8 Shiomi-cho, Choshi, Chiba 288-0025 (Japan); Chatake, Toshiyuki [Research Reactor Institute, Kyoto University, Asashironishi 2, Kumatori, Sennan, Osaka 590-0494 (Japan); Chiba-Kamoshida, Kaori [National Institute of Advanced Industrial Science and Technology (AIST), Umezono 1-1-1, Tsukuba, Ibaraki 305-8568 (Japan); Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki [Kurashiki University of Science and Arts, Nishinoura 2640, Tsurajima-cho, Kurashiki, Okayama 712-8505 (Japan); Yasuda, Ichiro [Faculty of Pharmaceutical Sciences, Chiba Institute of Science, 15-8 Shiomi-cho, Choshi, Chiba 288-0025 (Japan); Morimoto, Yukio [Research Reactor Institute, Kyoto University, Asashironishi 2, Kumatori, Sennan, Osaka 590-0494 (Japan); Faculty of Pharmaceutical Sciences, Chiba Institute of Science, 15-8 Shiomi-cho, Choshi, Chiba 288-0025 (Japan)

    2010-12-01

    Nattokinase, a protein found in high levels in the traditional Japanese food natto, has been reported to have high thrombolytic activity. In the present study, the crystallization of native nattokinase and the collection of X-ray diffraction date from a nattokinase crystal to a resolution of 1.74 Å are reported. Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27 724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a = 74.3, b = 49.9, c = 56.3 Å, β = 95.2°. Diffraction images were processed to a resolution of 1.74 Å with an R{sub merge} of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase.

  13. Preparation of single-crystal copper ferrite nanorods and nanodisks

    International Nuclear Information System (INIS)

    Du Jimin; Liu Zhimin; Wu Weize; Li Zhonghao; Han Buxing; Huang Ying

    2005-01-01

    This article, for the first time, reports the preparation of single-crystal copper ferrite nanorods and nanodisks. Using amorphous copper ferrite nanoparticles synthesized by reverse micelle as reaction precursor, single-crystal copper ferrite nanorods were synthesized via hydrothermal method in the presence of surfactant polyethylene glycol (PEG), however, copper ferrite nanodisks were prepared through the same procedures except the surfactant PEG. The resulting nanomaterials have been characterized by powder X-ray diffraction (XRD), selected electron area diffraction (SEAD), and transmission electron microscopy (TEM). The bulk composition of the samples was determined by means of X-ray photoelectron spectroscopy (XPS)

  14. Crystallized solids characterization by X-ray diffraction

    International Nuclear Information System (INIS)

    Broll, N.

    1996-01-01

    This work deals with the crystallized solids characterization by X-ray diffraction. The powders diffraction principle is described. Then are given the different powders diffraction experimental methods. An X-ray diffraction device is essentially constituted of three parts: the X-rays source, the sample and the detector. The source is usually constituted by an X-rays tube whereas the sample can be fixed on a photographic chamber or put on a goniometer. The different photographic chambers which can be used (Debye-Scherrer, Seeman-Bohlin and Guinier) are described. The powders diffractometer the most used is a Bragg-Brentano focusing diffractometer because it allows to obtain very sharp spectral lines and an important diffracted intensity. The detectors which are the mainly used are the scintillation counters. The most important use in powders diffractometry is the identification of the different phases of a sample. The phases identification consists to compare the unknown sample spectrum at those of standard materials indexed until now. Two methods exist at present. They are explained and their limits in the phases search are given. Another use of the X-ray diffraction is the quantitative analysis. It consists to determine the concentrations of each crystal phases of a sample. The principles of these quantitative methods are given. The lattice parameters of a polycrystal material can be determined from its X-ray pattern too with a very high precision. The way to index powders patterns is given. The residual stresses of materials can also be estimated. The principle of this measured method is explained. It is at last possible to study from an X-ray pattern, the material grain orientations during the different steps of preparation and working. (O.M.). 13 refs., 19 figs., 1 tab

  15. Validation of molecular crystal structures from powder diffraction data with dispersion-corrected density functional theory (DFT-D)

    DEFF Research Database (Denmark)

    van de Streek, Jacco; Neumann, Marcus A

    2014-01-01

    In 2010 we energy-minimized 225 high-quality single-crystal (SX) structures with dispersion-corrected density functional theory (DFT-D) to establish a quantitative benchmark. For the current paper, 215 organic crystal structures determined from X-ray powder diffraction (XRPD) data and published...

  16. An automatic control unit for A neutron diffraction crystal spectrometer

    International Nuclear Information System (INIS)

    Adib, M.; Abbas, Y.; Mostafa, M.; Hamouda, I.

    1982-01-01

    An automatic transistorized unit has been designed and constructed to control the operation of the double axis crystal spectrometer installed in front of one of the horizontal channels of the ET-RR-1 reactor. The function of the automatic unit is to store the diffracted neutrons at a certain angle with respect to the direction of the incident neutron beam in a selected channel of a 1024-multichannel analyzer for a certain preadjusted time period. AT the end of this time period the unit rotates the spectrometer's arm to another angle, selects the next channel of the MCA and provides the measurement of the diffracted neutron for the same time period. Such a sequence is repeated automatically over all angles required for the neutron diffraction pattern of the sample under investigation. As a result, the stored information at the MCA provides the neutron diffraction pattern as a function of channel number, where each channel corresponds to a certain scattering angle. The stored distribution at MCA can be obtained through the analyzer read out unit. The designed automatic unit has the possibility of providing the neutron diffraction pattern using a 6-digit scaler and a printer

  17. Automatic control unit for A neutron diffraction crystal spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Adib, M.; Abbas, Y.; Mostafa, M.; Hamouda, I.

    1982-01-01

    An automatic transistorized unit has been designed and constructed to control the operation of the double axis crystal spectrometer installed in front of one of the horizontal channels of the ET-RR-1 reactor. The function of the automatic unit is to store the diffracted neutrons at a certain angle with respect to the direction of the incident neutron beam in a selected channel of a 1024-multichannel analyzer for a certain preadjusted time period. AT the end of this time period the unit rotates the spectrometer's arm to another angle, selects the next channel of the MCA and provides the measurement of the diffracted neutron for the same time period. Such a sequence is repeated automatically over all angles required for the neutron diffraction pattern of the sample under investigation. As a result, the stored information at the MCA provides the neutron diffraction pattern as a function of channel number, where each channel corresponds to a certain scattering angle. The stored distribution at MCA can be obtained through the analyzer read out unit. The designed automatic unit has the possibility of providing the neutron diffraction pattern using a 6-digit scaler and a printer.

  18. Local layer structure of smectic liquid crystals by X-ray micro-diffraction

    CERN Document Server

    Takanishi, Y

    2003-01-01

    The local layer structure of smectic liquid crystal has been measured using time-resolved synchrotron X-ray micro-diffraction. Typical layer disorders observed in surface stabilized (anti-) ferroelectric liquid crystals, i.e. a stripe texture, a needed-like defect and a zigzag defect, are directly analyzed. The detailed analysis slows that the surface anchoring force due to the interaction between the liquid crystal molecule and the alignment thin film plays an important role to realize both the static and dynamic local layer structures. The layer structure of the circular domain observed in the liquid crystal of bent-shaped molecules found to depend on the applied electric field though the optical micrograph shows little difference. The frustrated, double and single layer structures of the bent-shaped molecule liquid crystal are determined depending on the terminal alkyl chain length. (author)

  19. Crystallization of porcine pancreatic elastase and a preliminary neutron diffraction experiment

    Energy Technology Data Exchange (ETDEWEB)

    Kinoshita, Takayoshi [Department of Biological Science, Graduate School of Science, Osaka Prefecture University, 1-1 Gakuen-cho, Naka-ku, Sakai, Osaka 599-8531 (Japan); Tamada, Taro [Molecular Structural Biology Group, Quantum Beam Science Directorate, Japan Atomic Energy Agency, 2-4 Shirakata-Shirane, Tokai, Ibaraki 319-1195 (Japan); Imai, Keisuke [Lead Discovery Research Laboratories, Astellas Pharma Inc., 21 Miyukigaoka, Tsukuba-shi, Ibaraki 305-8585 (Japan); Kurihara, Kazuo; Ohhara, Takashi [Molecular Structural Biology Group, Quantum Beam Science Directorate, Japan Atomic Energy Agency, 2-4 Shirakata-Shirane, Tokai, Ibaraki 319-1195 (Japan); Tada, Toshiji [Department of Biological Science, Graduate School of Science, Osaka Prefecture University, 1-1 Gakuen-cho, Naka-ku, Sakai, Osaka 599-8531 (Japan); Kuroki, Ryota, E-mail: kuroki.ryota@jaea.go.jp [Molecular Structural Biology Group, Quantum Beam Science Directorate, Japan Atomic Energy Agency, 2-4 Shirakata-Shirane, Tokai, Ibaraki 319-1195 (Japan); Department of Biological Science, Graduate School of Science, Osaka Prefecture University, 1-1 Gakuen-cho, Naka-ku, Sakai, Osaka 599-8531 (Japan)

    2007-04-01

    To investigate the structural characteristics of a covalent inhibitor bound to porcine pancreatic elastase (PPE), including H atoms and hydration by water, a crystal of porcine pancreatic elastase with its inhibitor was grown to a size of 1.6 mm{sup 3} for neutron diffraction study. The crystal diffracted to 2.3 Å resolution with sufficient quality for further structure determination owing to the similar atomic scattering properties of deuterium and carbon. Porcine pancreatic elastase (PPE) resembles the attractive drug target leukocyte elastase, which has been implicated in a number of inflammatory disorders. In order to investigate the structural characteristics of a covalent inhibitor bound to PPE, including H atoms and the hydration by water, a single crystal of PPE for neutron diffraction study was grown in D{sub 2}O containing 0.2 M sodium sulfate (pD 5.0) using the sitting-drop vapour-diffusion method. The crystal was grown to a size of 1.6 mm{sup 3} by repeated macroseeding. Neutron diffraction data were collected at room temperature using a BIX-3 diffractometer at the JRR-3 research reactor of the Japan Atomic Energy Agency (JAEA). The data set was integrated and scaled to 2.3 Å resolution in space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 51.2, b = 57.8, c = 75.6 Å.

  20. Iron single crystal growth from a lithium-rich melt

    Science.gov (United States)

    Fix, M.; Schumann, H.; Jantz, S. G.; Breitner, F. A.; Leineweber, A.; Jesche, A.

    2018-03-01

    α -Fe single crystals of rhombic dodecahedral habit were grown from a Li84N12Fe∼3 melt. Crystals of several millimeter along a side form at temperatures around T ≈ 800 ° C. Upon further cooling the growth competes with the formation of Fe-doped Li3N. The b.c.c. structure and good sample quality of α -Fe single crystals were confirmed by X-ray and electron diffraction as well as magnetization measurements and chemical analysis. A nitrogen concentration of 90 ppm was detected by means of carrier gas hot extraction. Scanning electron microscopy did not reveal any sign of iron nitride precipitates.

  1. Regio-Regular Oligo and Poly(3-hexyl thiophene): Precise Structural Markers from the Vibrational Spectra of Oligomer Single Crystals.

    KAUST Repository

    Brambilla, Luigi; Tommasini, Matteo; Botiz, Ioan; Rahimi, Khosrow; Agumba, John O.; Stingelin, Natalie; Zerbi, Giuseppe

    2014-01-01

    , namely, amorphous, semicrystalline, polycrystalline and single crystal. We have based our analysis on the spectra of the (3HT)8 single crystal (whose structure has been determined by selected area electron diffraction) taken as reference

  2. Reducing the positional modulation of NbO.sub.6./sub.-octahedra in Sr.sub.x./sub.Ba.sub.1-x./sub.Nb.sub.2./sub.O.sub.6./sub. by increasing the barium content: A single crystal neutron diffraction study at ambient temperature for x=0.61 and x=0.34

    Czech Academy of Sciences Publication Activity Database

    Schefer, J.; Schaniel, D.; Petříček, Václav; Woike, T.; Cousson, A.; Wöhlecke, M.

    2008-01-01

    Roč. 223, č. 6 (2008), s. 399-407 ISSN 0044-2968 R&D Projects: GA ČR GA202/06/0757 Institutional research plan: CEZ:AV0Z10100521 Keywords : influencing positional modulation * optical materials * modulated structure * single crystal structure analysis * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.708, year: 2008

  3. Patterning of Perovskite Single Crystals

    KAUST Repository

    Corzo, Daniel

    2017-06-12

    As the internet-of-things hardware integration continues to develop and the requirements for electronics keep diversifying and expanding, the necessity for specialized properties other than the classical semiconductor performance becomes apparent. The success of emerging semiconductor materials depends on the manufacturability and cost as much as on the properties and performance they offer. Solution-based semiconductors are an emerging concept that offers the advantage of being compatible with large-scale manufacturing techniques and have the potential to yield high-quality electronic devices at a lower cost than currently available solutions. In this work, patterns of high-quality MAPbBr3 perovskite single crystals in specific locations are achieved through the modification of the substrate properties and solvent engineering. The fabrication of the substrates involved modifying the surface adhesion forces through functionalization with self-assembled monolayers and patterning them by photolithography processes. Spin coating and blade coating were used to deposit the perovskite solution on the modified silicon substrates. While single crystal perovskites were obtained with the modification of substrates alone, solvent engineering helped with improving the Marangoni flows in the deposited droplets by increasing the contact angle and lowering the evaporation rate, therefore controlling and improving the shape of the grown perovskite crystals. The methodology is extended to other types of perovskites such as the transparent MAPbCl3 and the lead-free MABi2I9, demonstrating the adaptability of the process. Adapting the process to electrode arrays opened up the path towards the fabrication of optoelectronic devices including photodetectors and field-effect transistors, for which the first iterations are demonstrated. Overall, manufacturing and integration techniques permitting the fabrication of single crystalline devices, such as the method in this thesis work, are

  4. Magnetic structure of URhSi single crystal

    Czech Academy of Sciences Publication Activity Database

    Prokeš, K.; Andreev, Alexander V.; Honda, F.; Sechovský, V.

    2003-01-01

    Roč. 261, - (2003), s. 131-138 ISSN 0304-8853 R&D Projects: GA ČR GA202/02/0739 Institutional research plan: CEZ:AV0Z1010914 Keywords : URhSi single crystal * magnetization * neutron diffraction * magnetic structure determination Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.910, year: 2003

  5. A Medipix quantum area detector allows rotation electron diffraction data collection from submicrometre three-dimensional protein crystals

    Energy Technology Data Exchange (ETDEWEB)

    Nederlof, Igor; Genderen, Eric van; Li, Yao-Wang; Abrahams, Jan Pieter, E-mail: abrahams@chem.leidenuniv.nl [Leiden University, Einsteinweg 55, 2333 CC Leiden (Netherlands)

    2013-07-01

    An ultrasensitive Medipix2 detector allowed the collection of rotation electron-diffraction data from single three-dimensional protein nanocrystals for the first time. The data could be analysed using the standard X-ray crystallography programs MOSFLM and SCALA. When protein crystals are submicrometre-sized, X-ray radiation damage precludes conventional diffraction data collection. For crystals that are of the order of 100 nm in size, at best only single-shot diffraction patterns can be collected and rotation data collection has not been possible, irrespective of the diffraction technique used. Here, it is shown that at a very low electron dose (at most 0.1 e{sup −} Å{sup −2}), a Medipix2 quantum area detector is sufficiently sensitive to allow the collection of a 30-frame rotation series of 200 keV electron-diffraction data from a single ∼100 nm thick protein crystal. A highly parallel 200 keV electron beam (λ = 0.025 Å) allowed observation of the curvature of the Ewald sphere at low resolution, indicating a combined mosaic spread/beam divergence of at most 0.4°. This result shows that volumes of crystal with low mosaicity can be pinpointed in electron diffraction. It is also shown that strategies and data-analysis software (MOSFLM and SCALA) from X-ray protein crystallography can be used in principle for analysing electron-diffraction data from three-dimensional nanocrystals of proteins.

  6. A Medipix quantum area detector allows rotation electron diffraction data collection from submicrometre three-dimensional protein crystals

    International Nuclear Information System (INIS)

    Nederlof, Igor; Genderen, Eric van; Li, Yao-Wang; Abrahams, Jan Pieter

    2013-01-01

    An ultrasensitive Medipix2 detector allowed the collection of rotation electron-diffraction data from single three-dimensional protein nanocrystals for the first time. The data could be analysed using the standard X-ray crystallography programs MOSFLM and SCALA. When protein crystals are submicrometre-sized, X-ray radiation damage precludes conventional diffraction data collection. For crystals that are of the order of 100 nm in size, at best only single-shot diffraction patterns can be collected and rotation data collection has not been possible, irrespective of the diffraction technique used. Here, it is shown that at a very low electron dose (at most 0.1 e − Å −2 ), a Medipix2 quantum area detector is sufficiently sensitive to allow the collection of a 30-frame rotation series of 200 keV electron-diffraction data from a single ∼100 nm thick protein crystal. A highly parallel 200 keV electron beam (λ = 0.025 Å) allowed observation of the curvature of the Ewald sphere at low resolution, indicating a combined mosaic spread/beam divergence of at most 0.4°. This result shows that volumes of crystal with low mosaicity can be pinpointed in electron diffraction. It is also shown that strategies and data-analysis software (MOSFLM and SCALA) from X-ray protein crystallography can be used in principle for analysing electron-diffraction data from three-dimensional nanocrystals of proteins

  7. Synchrotron Bragg diffraction imaging characterization of synthetic diamond crystals for optical and electronic power device applications.

    Science.gov (United States)

    Tran Thi, Thu Nhi; Morse, J; Caliste, D; Fernandez, B; Eon, D; Härtwig, J; Barbay, C; Mer-Calfati, C; Tranchant, N; Arnault, J C; Lafford, T A; Baruchel, J

    2017-04-01

    Bragg diffraction imaging enables the quality of synthetic single-crystal diamond substrates and their overgrown, mostly doped, diamond layers to be characterized. This is very important for improving diamond-based devices produced for X-ray optics and power electronics applications. The usual first step for this characterization is white-beam X-ray diffraction topography, which is a simple and fast method to identify the extended defects (dislocations, growth sectors, boundaries, stacking faults, overall curvature etc. ) within the crystal. This allows easy and quick comparison of the crystal quality of diamond plates available from various commercial suppliers. When needed, rocking curve imaging (RCI) is also employed, which is the quantitative counterpart of monochromatic Bragg diffraction imaging. RCI enables the local determination of both the effective misorientation, which results from lattice parameter variation and the local lattice tilt, and the local Bragg position. Maps derived from these parameters are used to measure the magnitude of the distortions associated with polishing damage and the depth of this damage within the volume of the crystal. For overgrown layers, these maps also reveal the distortion induced by the incorporation of impurities such as boron, or the lattice parameter variations associated with the presence of growth-incorporated nitrogen. These techniques are described, and their capabilities for studying the quality of diamond substrates and overgrown layers, and the surface damage caused by mechanical polishing, are illustrated by examples.

  8. A 7 µm mini-beam improves diffraction data from small or imperfect crystals of macromolecules

    International Nuclear Information System (INIS)

    Sanishvili, Ruslan; Nagarajan, Venugopalan; Yoder, Derek; Becker, Michael; Xu, Shenglan; Corcoran, Stephen; Akey, David L.; Smith, Janet L.; Fischetti, Robert F.

    2008-01-01

    An X-ray mini-beam of 8 × 6 µm cross-section was used to collect diffraction data from protein microcrystals with volumes as small as 150–300 µm 3 . The benefits of the mini-beam for experiments with small crystals and with large inhomogeneous crystals are investigated. A simple apparatus for achieving beam sizes in the range 5-10 µm on a synchrotron beamline was implemented in combination with a small 125 × 25 µm focus. The resulting beam had sufficient flux for crystallographic data collection from samples smaller than 10 × 10 × 10 µm. Sample data were collected representing three different scenarios: (i) a complete 2.0 Å data set from a single strongly diffracting microcrystal, (ii) a complete and redundant 1.94 Å data set obtained by merging data from six microcrystals and (iii) a complete 2.24 Å data set from a needle-shaped crystal with less than 12 × 10 µm cross-section and average diffracting power. The resulting data were of high quality, leading to well refined structures with good electron-density maps. The signal-to-noise ratios for data collected from small crystals with the mini-beam were significantly higher than for equivalent data collected from the same crystal with a 125 × 25 µm beam. Relative to this large beam, use of the mini-beam also resulted in lower refined crystal mosaicities. The mini-beam proved to be advantageous for inhomogeneous large crystals, where better ordered regions could be selected by the smaller beam

  9. Crystals of DhaA mutants from Rhodococcus rhodochrous NCIMB 13064 diffracted to ultrahigh resolution: crystallization and preliminary diffraction analysis

    International Nuclear Information System (INIS)

    Stsiapanava, Alena; Koudelakova, Tana; Lapkouski, Mikalai; Pavlova, Martina; Damborsky, Jiri; Kuta Smatanova, Ivana

    2008-01-01

    Three mutants of the haloalkane dehalogenase DhaA derived from R. rhodochrous NCIMB 13064 were crystallized and diffracted to ultrahigh resolution. The enzyme DhaA from Rhodococcus rhodochrous NCIMB 13064 belongs to the haloalkane dehalogenases, which catalyze the hydrolysis of haloalkanes to the corresponding alcohols. The haloalkane dehalogenase DhaA and its variants can be used to detoxify the industrial pollutant 1,2,3-trichloropropane (TCP). Three mutants named DhaA04, DhaA14 and DhaA15 were constructed in order to study the importance of tunnels connecting the buried active site with the surrounding solvent to the enzymatic activity. All protein mutants were crystallized using the sitting-drop vapour-diffusion method. The crystals of DhaA04 belonged to the orthorhombic space group P2 1 2 1 2 1 , while the crystals of the other two mutants DhaA14 and DhaA15 belonged to the triclinic space group P1. Native data sets were collected for the DhaA04, DhaA14 and DhaA15 mutants at beamline X11 of EMBL, DESY, Hamburg to the high resolutions of 1.30, 0.95 and 1.15 Å, respectively

  10. Flat liquid crystal diffractive lenses with variable focus and magnification

    Science.gov (United States)

    Valley, Pouria

    Non-mechanical variable lenses are important for creating compact imaging devices. Various methods employing dielectrically actuated lenses, membrane lenses, and liquid crystal lenses were previously proposed [1-4]. In This dissertation the design, fabrication, and characterization of innovative flat tunable-focus liquid crystal diffractive lenses (LCDL) are presented. LCDL employ binary Fresnel zone electrodes fabricated on Indium-Tin-Oxide using conventional micro-photolithography. The light phase can be adjusted by varying the effective refractive index of a nematic liquid crystal sandwiched between the electrodes and a reference substrate. Using a proper voltage distribution across various electrodes the focal length can be changed between several discrete values. Electrodes are shunted such that the correct phase retardation step sequence is achieved. If the number of 2pi zone boundaries is increased by a factor of m the focal length is changed from f to f/m based on the digitized Fresnel zone equation: f = rm2/2mlambda, where r m is mth zone radius, and lambda is the wavelength. The chromatic aberration of the diffractive lens is addressed and corrected by adding a variable fluidic lens. These LCDL operate at very low voltage levels (+/-2.5V ac input), exhibit fast switching times (20-150 ms), can have large apertures (>10 mm), and small form factor, and are robust and insensitive to vibrations, gravity, and capillary effects that limit membrane and dielectrically actuated lenses. Several tests were performed on the LCDL including diffraction efficiency measurement, switching dynamics, and hybrid imaging with a refractive lens. Negative focal lengths are achieved by adjusting the voltages across electrodes. Using these lenses in combination, magnification can be changed and zoom lenses can be formed. These characteristics make LCDL a good candidate for a variety of applications including auto-focus and zoom lenses in compact imaging devices such as camera

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

    Energy Technology Data Exchange (ETDEWEB)

    Fan, D.; Luo, S. N., E-mail: sluo@pims.ac.cn [The Peac Institute of Multiscale Sciences, Chengdu, Sichuan 610031 (China); Key Laboratory of Advanced Technologies of Materials, Ministry of Education, Southwest Jiaotong University, Chengdu, Sichuan 610031 (China); Huang, J. W.; Zeng, X. L.; Li, Y.; E, J. C.; Huang, J. Y. [The Peac Institute of Multiscale Sciences, Chengdu, Sichuan 610031 (China); Sun, T.; Fezzaa, K. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Wang, Z. [Physics Division P-25, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States)

    2016-05-15

    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 quantify 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.

  12. Regularities of recrystallization in rolled Zr single crystals

    International Nuclear Information System (INIS)

    Isaenkova, M; Perlovich, Yu; Fesenko, V; Krymskaya, O; Krapivka, N; Thu, S S

    2015-01-01

    Experiments by rolled single crystals give a more visible conception of the operating mechanisms of plastic deformation and the following recrystallization, than experiments by polycrystals. Studies by usage of X-ray diffraction methods were conducted by Zr single crystals. It was revealed, that regions of the α-Zr matrix, deformed mainly by twinning, are characterized with decreased tendency to recrystallization. Orientations of recrystallized α-Zr grains correspond to “slopes” of maxima in the rolling texture, where the level of crystalline lattice distortion is maximal and the number of recrystallization nuclei is most of all. (paper)

  13. Laser induced single-crystal transition in polycrystalline silicon

    International Nuclear Information System (INIS)

    Vitali, G.; Bertolotti, M.; Foti, G.; Rimini, E.

    1978-01-01

    Transition to single crystal of polycrystalline Si material underlying a Si crystal substrate of 100 orientation was obtained via laser irradiation. The changes in the structure were analyzed by reflection high energy electron diffraction and by channeling effect technique using 2.0 MeV He Rutherford scattering. The power density required to induce the transition in a 4500 A thick polycrystalline layer is about 70 MW/cm 2 (50ns). The corresponding amorphous to single transition has a threshold of about 45 MW/cm 2 . (orig.) 891 HPOE [de

  14. Principles of crystallization, and methods of single crystal growth

    International Nuclear Information System (INIS)

    Chacra, T.

    2010-01-01

    Most of single crystals (monocrystals), have distinguished optical, electrical, or magnetic properties, which make from single crystals, key elements in most of technical modern devices, as they may be used as lenses, Prisms, or grating sin optical devises, or Filters in X-Ray and spectrographic devices, or conductors and semiconductors in electronic, and computer industries. Furthermore, Single crystals are used in transducer devices. Moreover, they are indispensable elements in Laser and Maser emission technology.Crystal Growth Technology (CGT), has started, and developed in the international Universities and scientific institutions, aiming at some of single crystals, which may have significant properties and industrial applications, that can attract the attention of international crystal growth centers, to adopt the industrial production and marketing of such crystals. Unfortunately, Arab universities generally, and Syrian universities specifically, do not give even the minimum interest, to this field of Science.The purpose of this work is to attract the attention of Crystallographers, Physicists and Chemists in the Arab universities and research centers to the importance of crystal growth, and to work on, in the first stage to establish simple, uncomplicated laboratories for the growth of single crystal. Such laboratories can be supplied with equipment, which are partly available or can be manufactured in the local market. Many references (Articles, Papers, Diagrams, etc..) has been studied, to conclude the most important theoretical principles of Phase transitions,especially of crystallization. The conclusions of this study, are summarized in three Principles; Thermodynamic-, Morphologic-, and Kinetic-Principles. The study is completed by a brief description of the main single crystal growth methods with sketches, of equipment used in each method, which can be considered as primary designs for the equipment, of a new crystal growth laboratory. (author)

  15. Production, crystallization and preliminary X-ray diffraction analysis of the allergen Can f 2 from Canis familiaris

    International Nuclear Information System (INIS)

    Madhurantakam, Chaithanya; Nilsson, Ola B.; Jönsson, Klas; Grönlund, Hans; Achour, Adnane

    2009-01-01

    The recombinant form of the allergen Can f 2 from C. familiaris was produced, isolated and crystallized in two different forms. Preliminary X-ray diffraction analyses are reported for the two crystal forms of Can f 2. The allergen Can f 2 from dog (Canis familiaris) present in saliva, dander and fur is an important cause of allergic sensitization worldwide. Here, the production, isolation, crystallization and preliminary X-ray diffraction analysis of two crystal forms of recombinant Can f 2 are reported. The first crystal form belonged to space group C222, with unit-cell parameters a = 68.7, b = 77.3, c = 65.1 Å, and diffracted to 1.55 Å resolution, while the second crystal form belonged to space group C2, with unit-cell parameters a = 75.7, b = 48.3, c = 68.7 Å, β = 126.5°, and diffracted to 2.1 Å resolution. Preliminary data analysis indicated the presence of a single molecule in the asymmetric unit for both crystal forms

  16. Interpretation of the shape of electron diffraction spots from small polyhedral crystals by means of the crystal shape amplitude

    International Nuclear Information System (INIS)

    Neumann, W.; Hofmeister, H.; Heydenreich, J.; Komrska, J.

    1988-01-01

    The influence of the crystal shape on the fine structure of transmission electron diffraction (TED) patterns described by the crystal shape amplitude is discussed. A general algebraic expression for the crystal shape amplitude of any crystal polyhedron is used for computing the intensity distribution of TED reflections. The computer simulation method is applied to the analysis of the fine structure of TED patterns of small gold and palladium crystals having octahedral and tetrahedral habits. (orig.)

  17. Electrically Anisotropic Layered Perovskite Single Crystal

    KAUST Repository

    Li, Ting-You

    2016-01-01

    -23). However, the difficulty in growing large-sized LOIHPs single crystal with superior electrical properties limits their practical applications. Here, we report a method to grow the centimeter-scaled LOIHP single crystal of [(HOC2H4NH3)2PbI4], demonstrating

  18. Confinement stabilises single crystal vaterite rods.

    OpenAIRE

    Schenk, AS; Albarracin, EJ; Kim, YY; Ihli, J; Meldrum, FC

    2014-01-01

    Single-crystals of vaterite, the least-stable anhydrous polymorph of CaCO3, are rare in biogenic and synthetic systems. We here describe the synthesis of high aspect ratio single crystal vaterite rods under additive-free conditions by precipitating CaCO3 within the cylindrical pores of track-etch membranes.

  19. Single Crystal Synthesis and STM Studies of High Temperature Superconductors

    Science.gov (United States)

    Barrientos, Alfonso

    1997-01-01

    This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

  20. Reconstructing an icosahedral virus from single-particle diffraction experiments

    Science.gov (United States)

    Saldin, D. K.; Poon, H.-C.; Schwander, P.; Uddin, M.; Schmidt, M.

    2011-08-01

    The first experimental data from single-particle scattering experiments from free electron lasers (FELs) are now becoming available. The first such experiments are being performed on relatively large objects such as viruses, which produce relatively low-resolution, low-noise diffraction patterns in so-called ``diffract-and-destroy'' experiments. We describe a very simple test on the angular correlations of measured diffraction data to determine if the scattering is from an icosahedral particle. If this is confirmed, the efficient algorithm proposed can then combine diffraction data from multiple shots of particles in random unknown orientations to generate a full 3D image of the icosahedral particle. We demonstrate this with a simulation for the satellite tobacco necrosis virus (STNV), the atomic coordinates of whose asymmetric unit is given in Protein Data Bank entry 2BUK.

  1. Single photon energy dispersive x-ray diffraction

    International Nuclear Information System (INIS)

    Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando; Suggit, Matthew J.; Wark, Justin S.; Hawreliak, James A.; Collins, Gilbert W.; Coppari, Federica; Eggert, Jon H.; Tang, Henry

    2014-01-01

    With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signal from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored

  2. Single photon energy dispersive x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando; Suggit, Matthew J.; Wark, Justin S. [Department of Physics, Clarendon Laboratory, University of Oxford, Parks Road, Oxford OX1 3PU (United Kingdom); Hawreliak, James A.; Collins, Gilbert W.; Coppari, Federica; Eggert, Jon H. [Lawrence Livermore National Laboratory, Livermore, California 94551 (United States); Tang, Henry [Department of Earth and Planetary Science, University of California Berkeley, Berkeley, California 94720 (United States)

    2014-03-15

    With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signal from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored.

  3. Growth of emerald single crystals

    International Nuclear Information System (INIS)

    Bukin, G.V.; Godovikov, A.A.; Klyakin, V.A.; Sobolev, V.S.

    1986-01-01

    In addition to its use for jewelry, emerald can also be used in low-noise microwave amplifiers. The authors discuss flux crystallization of emerald and note that when emerald is grown by this method, it is desirable to use solvents which dissolve emerald with minimum deviations from congruence but at the same time with sufficient high efficiency. Emerald synthesis and crystal growth from slowly cooled solutions is discussed as another possibility. The techniques are examined. Vapor synthesis and growht of beryl crystals re reviewed and the authors experimentally study the seeded CVD crystallization of beryl from BeO, Al 2 O 3 and SiO 2 oxides, by using complex compounds as carrier agents. The color of crystals of emerald and other varieties of beryl is detemined by slelective light absorption in teh visible part of the spectrum and depends on the density and structural positions of chromphore ions: chromium, iron, vanadium, nickel, manganese and cobalt

  4. Expression, purification, crystallization and preliminary diffraction studies of the mammalian DAG kinase homologue YegS from Escherichia coli

    International Nuclear Information System (INIS)

    Bakali H, M. Amin; Nordlund, Pär; Hallberg, B. Martin

    2006-01-01

    The overexpression, crystallization and preliminary diffraction analysis of E. coli YegS are reported. yegS is a gene encoding a 32 kDa cytosolic protein with unknown function but with strong sequence homology to a family of structurally uncharacterized eukaryotic non-protein kinases: diacylglycerol kinases, sphingosine kinases and ceramide kinases. Here, the overexpression, crystallization and preliminary diffraction analysis of Escherichia coli YegS are reported. The crystals belong to space group P2 1 , with unit-cell parameters a = 42.4, b = 166.1, c = 48.5 Å, β = 96.97°. The presence of a dimer in the asymmetric unit was estimated to give a Matthews coefficient (V M ) of 2.5 Å 3 Da −1 and a solvent content of 50.8%(v/v). Single-wavelength diffraction data were collected to a resolution of 1.9 Å using synchrotron radiation

  5. Ion implantation induced blistering of rutile single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Xiang, Bing-Xi [School of Physics, Shandong University, Jinan, Shandong 250100 (China); Jiao, Yang [College of Physics and Electronics, Shandong Normal University, Jinan, Shandong 250100 (China); Guan, Jing [School of Physics, Shandong University, Jinan, Shandong 250100 (China); Wang, Lei [School of Physics, Shandong University, Jinan, Shandong 250100 (China); Key Laboratory of Nanodevices and Applications, Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese Academy of Sciences (China)

    2015-07-01

    The rutile single crystals were implanted by 200 keV He{sup +} ions with a series fluence and annealed at different temperatures to investigate the blistering behavior. The Rutherford backscattering spectrometry, optical microscope and X-ray diffraction were employed to characterize the implantation induced lattice damage and blistering. It was found that the blistering on rutile surface region can be realized by He{sup +} ion implantation with appropriate fluence and the following thermal annealing.

  6. Crystal structure and magnetic susceptibility of UOSe single crystals

    International Nuclear Information System (INIS)

    Kaczorowski, D.; Muenster Univ.; Poettgen, R.; Jeitschko, W.; Gajek, Z.; Zygmunt, A.

    1993-01-01

    The crystal structure and magnetic susceptibility behaviour of UOSe single crystals have been studied. UOSe crystalizes in the tetragonal PbFC1-type structure (space group P4/nmm) with the lattice parameters: a = 390.38(5) pm and c = 698.05(9) pm. It orders antiferromagnetically at T N =100±2 K and exhibits a very strong anisotropy in the susceptibility vs temperature variation. The magnetic and thermodynamic properties of UOSe are successfully interpreted in the framework of a perturbative ab initio crystal field approach. (Author)

  7. Crystal structure and magnetic susceptibility of UOSe single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Kaczorowski, D. (Polish Academy of Sciences, Wroclaw (Poland). Inst. for Low Temperature and Structure Research Muenster Univ. (Germany). Anorganisch-Chemisches Inst.); Poettgen, R.; Jeitschko, W. (Muenster Univ. (Germany). Anorganisch-Chemisches Inst.); Gajek, Z.; Zygmunt, A. (Polish Academy of Sciences, Wroclaw (Poland). Inst. for Low Temperature and Structure Research)

    1993-01-01

    The crystal structure and magnetic susceptibility behaviour of UOSe single crystals have been studied. UOSe crystalizes in the tetragonal PbFC1-type structure (space group P4/nmm) with the lattice parameters: a = 390.38(5) pm and c = 698.05(9) pm. It orders antiferromagnetically at T[sub N]=100[+-]2 K and exhibits a very strong anisotropy in the susceptibility vs temperature variation. The magnetic and thermodynamic properties of UOSe are successfully interpreted in the framework of a perturbative ab initio crystal field approach. (Author).

  8. Crystal growth and characterization of new semiorganic nonlinear optical single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Kulshrestha, Shobha, E-mail: shobha011986@gmail.com; Shrivastava, A. K., E-mail: ashwaniaks@rediffmail.com [School of Studies in Physics, Jiwaji University Gwalior (M.P.) – 474 011 (India)

    2016-05-06

    An organic material of a L-histidine monohydrochloride single crystal was grown in a distilled water solution using the slow evaporation method at 40–45°C. The grown crystal was transparent and colourless, with a size of about 20 × 9 × 5 mm{sup 3}, obtained within a period of 21 days. The solubility of grown crystals have found out at various temperatures. The UV-visible transmittance studies show that the grown crystals have wide optical transparency in the entire visible region It is observed that the crystal has transparency window from 255nm to 700nm and its energy gap (Eg) found to be is 3.1eV. The grown crystal was subjected to powder X-ray diffraction analysis, confirming that the orthorhombic crystalline nature of the crystal. To identify the surface morphology, the as grown crystal was subjected to FE-SEM technique. The chemical composition of the grown crystal was estimated by Energy dispersive X-ray analysis. The optical behaviour of the grown crystal was analyzed by PL study.

  9. Growth and characterization of nonlinear optical single crystal: Nicotinic L-tartaric

    Energy Technology Data Exchange (ETDEWEB)

    Sheelarani, V.; Shanthi, J., E-mail: shanthinelson@gmail.com [Department of Physics, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore-641043 (India)

    2015-06-24

    Nonlinear optical single crystals were grown from Nicotinic and L-Tartaric acid by slow evaporation technique at room temperature. Structure of the grown crystal was confirmed by single crystal X-ray diffraction studies, The crystallinity of the Nicotinic L-Tartaric (NLT) crystals was confirmed from the powder XRD pattern. The transparent range and cut off wavelength of the grown crystal was studied by the UV–Vis spectroscopic analysis.The thermal stability of the crystal was studied by TG-DTA. The second harmonic generation (SHG) efficiency of NLT was confirmed by Kurtz Perry technique.

  10. Relaxor-PT Single Crystal Piezoelectric Sensors

    Directory of Open Access Journals (Sweden)

    Xiaoning Jiang

    2014-07-01

    Full Text Available Relaxor-PbTiO3 piezoelectric single crystals have been widely used in a broad range of electromechanical devices, including piezoelectric sensors, actuators, and transducers. This paper reviews the unique properties of these single crystals for piezoelectric sensors. Design, fabrication and characterization of various relaxor-PT single crystal piezoelectric sensors and their applications are presented and compared with their piezoelectric ceramic counterparts. Newly applicable fields and future trends of relaxor-PT sensors are also suggested in this review paper.

  11. LCP crystallization and X-ray diffraction analysis of VcmN, a MATE transporter from Vibrio cholerae

    Energy Technology Data Exchange (ETDEWEB)

    Kusakizako, Tsukasa [Graduate School of Science, The University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo 113-0032 (Japan); Tanaka, Yoshiki [Graduate School of Biological Sciences, Nara Institute of Science and Technology, 8916-5 Takayama-cho, Ikoma, Nara 630-0192 (Japan); Hipolito, Christopher J. [Graduate School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); University of Tsukuba, 1-1-1 Tennodai, Tsukuba 305-8575 (Japan); Kuroda, Teruo [Graduate School of Biomedical and Health Sciences, Hiroshima University, 1-2-3 Kasumi, Minami-ku, Hiroshima 734-8553 (Japan); Ishitani, Ryuichiro [Graduate School of Science, The University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo 113-0032 (Japan); Suga, Hiroaki [Graduate School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); Nureki, Osamu, E-mail: nureki@bs.s.u-tokyo.ac.jp [Graduate School of Science, The University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo 113-0032 (Japan)

    2016-06-22

    A V. cholerae MATE transporter was crystallized using the lipidic cubic phase (LCP) method. X-ray diffraction data sets were collected from single crystals obtained in a sandwich plate and a sitting-drop plate to resolutions of 2.5 and 2.2 Å, respectively. Multidrug and toxic compound extrusion (MATE) transporters, one of the multidrug exporter families, efflux xenobiotics towards the extracellular side of the membrane. Since MATE transporters expressed in bacterial pathogens contribute to multidrug resistance, they are important therapeutic targets. Here, a MATE-transporter homologue from Vibrio cholerae, VcmN, was overexpressed in Escherichia coli, purified and crystallized in lipidic cubic phase (LCP). X-ray diffraction data were collected to 2.5 Å resolution from a single crystal obtained in a sandwich plate. The crystal belonged to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 52.3, b = 93.7, c = 100.2 Å. As a result of further LCP crystallization trials, crystals of larger size were obtained using sitting-drop plates. X-ray diffraction data were collected to 2.2 Å resolution from a single crystal obtained in a sitting-drop plate. The crystal belonged to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 61.9, b = 91.8, c = 100.9 Å. The present work provides valuable insights into the atomic resolution structure determination of membrane transporters.

  12. Growth and microtopographic study of CuInSe{sub 2} single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Chauhan, Sanjaysinh M.; Chaki, Sunil, E-mail: sunilchaki@yahoo.co.in; Deshpande, M. P. [Department of Physics, Sardar Patel University, Vallabh Vidyanagar, Gujarat - 388120 (India); Tailor, J. P. [Applied Physics Department, S.V.N.I.T., Surat, Gujarat - 395007 (India)

    2016-05-23

    The CuInSe{sub 2} single crystals were grown by chemical vapour transport (CVT) technique using iodine as transporting agent. The elemental composition of the as-grown CuInSe{sub 2} single crystals was determined by energy dispersive analysis of X-ray (EDAX). The unit cell crystal structure and lattice parameters were determined by X-ray diffraction (XRD) technique. The surface microtopographic study of the as-grown CuInSe{sub 2} single crystals surfaces were done to study the defects, growth mechanism, etc. of the CVT grown crystals.

  13. Crystallization and preliminary X-ray diffraction analysis of recombinant hepatitis E virus-like particle

    International Nuclear Information System (INIS)

    Wang, Che-Yen; Miyazaki, Naoyuki; Yamashita, Tetsuo; Higashiura, Akifumi; Nakagawa, Atsushi; Li, Tian-Cheng; Takeda, Naokazu; Xing, Li; Hjalmarsson, Erik; Friberg, Claes; Liou, Der-Ming; Sung, Yen-Jen; Tsukihara, Tomitake; Matsuura, Yoshiharu; Miyamura, Tatsuo; Cheng, R. Holland

    2008-01-01

    A recombinant virus-like particle that is a potential oral hepatitis E vaccine was crystallized. Diffraction data were collected to 8.3 Å resolution and the X-ray structure was phased with the aid of a low-resolution density map determined using cryo-electron microscopy data. Hepatitis E virus (HEV) accounts for the majority of enterically transmitted hepatitis infections worldwide. Currently, there is no specific treatment for or vaccine against HEV. The major structural protein is derived from open reading frame (ORF) 2 of the viral genome. A potential oral vaccine is provided by the virus-like particles formed by a protein construct of partial ORF3 protein (residue 70–123) fused to the N-terminus of the ORF2 protein (residues 112–608). Single crystals obtained by the hanging-drop vapour-diffusion method at 293 K diffract X-rays to 8.3 Å resolution. The crystals belong to space group P2 1 2 1 2 1 , with unit-cell parameters a = 337, b = 343, c = 346 Å, α = β = γ = 90°, and contain one particle per asymmetric unit

  14. Moessbauer radiation dynamical diffraction in crystals being subjected to the action of external variable fields

    International Nuclear Information System (INIS)

    Baryshevskii, V.G.; Skadorov, V.V.

    1986-01-01

    A dynamical theory is developed of the Moessbauer radiation diffraction by crystals being subjected to an variable external field action. Equations describing the dynamical diffraction by nonstationary crystals are obtained. It is shown that the resonant interaction between Moessbauer radiation and shift field induced in the crystal by a variable external field giving rise to an effective conversion of the incident wave into a wave with changed frequency. (author)

  15. The bent crystal diffraction spectrometer at the BR2 reactor in Mol

    Science.gov (United States)

    Kaerts, E.; Jacobs, L.; Vandenput, G.; Van Assche, P. H. M.

    1988-05-01

    The DuMond-type bent crystal diffraction spectrometer installed at the BR2 reactor in Mol is presented. The spectrometer is mainly designed to study nuclear γ-transitions following thermal neutron capture. It covers the energy interval 25 ≦ Eγ ≦ 1500 keV. Instead of the traditionally used quartz crystals, a highly perfect silicium crystal is chosen as analysing crystal. Diffraction occurs from the (220) plane. The "quasi-mosaic" width, introduced by bending the crystal, is as small as 0.2″. The integrated reflecting power R of the bent crystal stays constant up to 1.5 MeV in first, 680 keV in second and 300 keV in third diffraction order. For higher photon energies, only an E-1 energy dependence is observed in second and third diffraction order. Consequently, besides improving the energy resolution, the use of these silicium crystals substantially increases the spectrometer efficiency and extends the high energy limit of bent crystal diffraction spectrometers. The diffraction angles are measured with a symmetrical interferometer system which covers an angular range of -6° to +6° with a precision of about 0.01″. Minimum diffraction line widths of 0.9″ have been measured, corresponding to an energy resolution ΔE = 1.35 × 10 -6E2n-1 keV -1. The dominant contribution to the observed line widths arises from the finite extent of the source.

  16. Refinement of the crystal structure of malachite, Cu2(OH)2CO3, by neutron diffraction

    International Nuclear Information System (INIS)

    Zigan, F.; Joswig, W.; Schuster, H.D.; Mason, S.A.

    1977-01-01

    The crystal structure of malachite is refined (R = 0,021) with the intensity values of 635 independent neutron reflexions from a single crystal, rather free from absorption and extinction. Concerning the structural geometry, no essential deviations occur from the known results of x-ray diffraction. The thermal elongations are generally largest about the normal to the (201) layers, between which the bonding is relatively weak. In both of the (medium, bent) OH...O hydrogen bonds, the anisotropic thermal parameters, converted according to the riding model, are - with certain restrictions - in agreement with the measured infrared spectrum as well as with frequencies and directions of the proton vibration calculated from the bonding geometry on the basis of a theoretical model. (orig.) [de

  17. Coherent diffractive imaging of solid state reactions in zinc oxide crystals

    Science.gov (United States)

    Leake, Steven J.; Harder, Ross; Robinson, Ian K.

    2011-11-01

    We investigated the doping of zinc oxide (ZnO) microcrystals with iron and nickel via in situ coherent x-ray diffractive imaging (CXDI) in vacuum. Evaporated thin metal films were deposited onto the ZnO microcrystals. A single crystal was selected and tracked through annealing cycles. A solid state reaction was observed in both iron and nickel experiments using CXDI. A combination of the shrink wrap and guided hybrid-input-output phasing methods were applied to retrieve the electron density. The resolution was 33 nm (half order) determined via the phase retrieval transfer function. The resulting images are nevertheless sensitive to sub-angstrom displacements. The exterior of the microcrystal was found to degrade dramatically. The annealing of ZnO microcrystals coated with metal thin films proved an unsuitable doping method. In addition the observed defect structure of one crystal was attributed to the presence of an array of defects and was found to change upon annealing.

  18. Single-crystal X-ray diffraction study of Cs{sub 2}Er[Si{sub 6}O{sub 14}]F and Cs{sub 2}Er[Si{sub 4}O{sub 10}]F

    Energy Technology Data Exchange (ETDEWEB)

    Dabic, Predrag; Kremenovic, Aleksandar; Vulic, Predag [Belgrade Univ. (Serbia). Lab. of Crystallography; Kahlenberg, Volker; Schmidmair, Daniela [Innsbruck Univ. (Austria). Inst. of Mineralogy and Petrography

    2016-07-01

    Single-crystal growth experiments in the system CsF-Er{sub 2}O{sub 3}-SiO{sub 2} resulted in the simultaneous crystallization of two chemically related compounds within the same run: Cs{sub 2}Er[Si{sub 6}O{sub 14}]F (phase I) and Cs{sub 2}Er[Si{sub 4}O{sub 10}]F (phase II). They represent the first examples for cesium erbium silicates containing fluorine. Basic crystallographic data are - phase I: space group Cmca, a=17.2556(6) Aa, b=24.6565(7) Aa, c=14.4735(5) Aa, V=6157.9(3) Aa{sup 3}, Z=16; phase II: space group Pnma, a=22.3748(7) Aa, b=8.8390(2) Aa, c=11.9710(4) Aa, V=2367.5(1) Aa{sup 3}, Z=8. The structures were determined by direct methods and refined to residuals of R(vertical stroke F vertical stroke)=0.0229 for 2920 (phase I) and 0.0231 for 2314 (phase II) independent observed reflections with I>2σ(I). The structure of phase I represents a previously unknown structure type with a three dimensional tetrahedral framework consisting of Q{sup 3} and Q{sup 4} groups in the ratio 2:1. Basic building units of the network are unbranched sechser single-chains running parallel to [001]. The network can be conveniently built up from the condensation of tetrahedral layers parallel to (010) or (100), respectively. The crystal structure of phase II can be classified as a tubular or columnar chain silicate indicating that the backbones of the structure are multiple chains of silicate tetrahedra. This structure is isotypic to a Cs{sub 2}Y[Si{sub 4}O{sub 10}]F, a compound that has been characterized previously. Alternatively, both compounds can be described as mixed octahedral-tetrahedral frameworks, which can be classified according to their polyhedral microensembles. A topological analysis of both nets is presented.

  19. Hydrogen positions in single nanocrystals revealed by electron diffraction

    Czech Academy of Sciences Publication Activity Database

    Palatinus, Lukáš; Brázda, Petr; Boullay, P.; Pérez, O.; Klementová, Mariana; Petit, S.; Eigner, Václav; Zaarour, M.; Mintova, S.

    2017-01-01

    Roč. 355, č. 6321 (2017), s. 166-169 ISSN 0036-8075 R&D Projects: GA ČR GA16-10035S; GA MŠk LO1603 EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : hydrogen atoms * crystal structure * electron diffraction tomography * nanocrystalline materials Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 37.205, year: 2016

  20. Measurement of the velocity of sound in crystals by pulsed neutron diffraction

    International Nuclear Information System (INIS)

    Willis, B.T.M.; Carlile, C.J.; Ward, R.C.; David, W.I.F.; Johnson, M.W.

    1986-03-01

    The diffraction method of observing elementary excitations in crystals has been applied to the study of one-phonon thermal diffuse scattering from pyrolytic graphite on a high resolution pulsed neutron diffractometer. The variation of the phase velocity of sound as a function of direction in the crystal and efficient method of determining sound velocities in crystals under extreme conditions. (author)

  1. Classification using diffraction patterns for single-particle analysis

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Hongli; Zhang, Kaiming [Department of Biophysics, the Health Science Centre, Peking University, Beijing 100191 (China); Meng, Xing, E-mail: xmeng101@gmail.com [Wadsworth Centre, New York State Department of Health, Albany, New York 12201 (United States)

    2016-05-15

    An alternative method has been assessed; diffraction patterns derived from the single particle data set were used to perform the first round of classification in creating the initial averages for proteins data with symmetrical morphology. The test protein set was a collection of Caenorhabditis elegans small heat shock protein 17 obtained by Cryo EM, which has a tetrahedral (12-fold) symmetry. It is demonstrated that the initial classification on diffraction patterns is workable as well as the real-space classification that is based on the phase contrast. The test results show that the information from diffraction patterns has the enough details to make the initial model faithful. The potential advantage using the alternative method is twofold, the ability to handle the sets with poor signal/noise or/and that break the symmetry properties. - Highlights: • New classification method. • Create the accurate initial model. • Better in handling noisy data.

  2. Classification using diffraction patterns for single-particle analysis

    International Nuclear Information System (INIS)

    Hu, Hongli; Zhang, Kaiming; Meng, Xing

    2016-01-01

    An alternative method has been assessed; diffraction patterns derived from the single particle data set were used to perform the first round of classification in creating the initial averages for proteins data with symmetrical morphology. The test protein set was a collection of Caenorhabditis elegans small heat shock protein 17 obtained by Cryo EM, which has a tetrahedral (12-fold) symmetry. It is demonstrated that the initial classification on diffraction patterns is workable as well as the real-space classification that is based on the phase contrast. The test results show that the information from diffraction patterns has the enough details to make the initial model faithful. The potential advantage using the alternative method is twofold, the ability to handle the sets with poor signal/noise or/and that break the symmetry properties. - Highlights: • New classification method. • Create the accurate initial model. • Better in handling noisy data.

  3. Defect free single crystal thin layer

    KAUST Repository

    Elafandy, Rami Tarek Mahmoud

    2016-01-28

    A gallium nitride film can be a dislocation free single crystal, which can be prepared by irradiating a surface of a substrate and contacting the surface with an etching solution that can selectively etch at dislocations.

  4. Defect free single crystal thin layer

    KAUST Repository

    Elafandy, Rami Tarek Mahmoud; Ooi, Boon S.

    2016-01-01

    A gallium nitride film can be a dislocation free single crystal, which can be prepared by irradiating a surface of a substrate and contacting the surface with an etching solution that can selectively etch at dislocations.

  5. Studies on growth, crystal structure and characterization of novel organic nicotinium trifluoroacetate single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Dhanaraj, P.V. [Centre for Crystal Growth, SSN College of Engineering, Kalavakkam 603 110 (India); Rajesh, N.P., E-mail: rajeshnp@hotmail.com [Centre for Crystal Growth, SSN College of Engineering, Kalavakkam 603 110 (India); Sundar, J. Kalyana; Natarajan, S. [Department of Physics, Madurai Kamaraj University, Madurai 625 021 (India); Vinitha, G. [Department of Physics, Crescent Engineering College, Chennai 600 048 (India)

    2011-09-15

    Highlights: {yields} Good quality crystals of nicotinium trifluoroacetate in monoclinic system were grown for first time. {yields} Nicotinium trifluoroacetate crystal exhibits third order nonlinear optical properties. {yields} The optical spectrum of nicotinium trifluoroacetate crystal reveals the wide transmission in the entire range with cutoff wavelength at 286 nm. {yields} Nicotinium trifluoroacetate is a low dielectric constant material. - Abstract: An organic material, nicotinium trifluoroacetate (NTF) was synthesized and single crystals in monoclinic system were grown from aqueous solution for the first time. Its solubility and metastable zone width were estimated. The crystal structure of NTF was analyzed to reveal the molecular arrangements and the formation of hydrogen bonds in the crystal. High-resolution X-ray diffraction rocking curve measurements were performed to analyze the structural perfection of the grown crystals. Functional groups in NTF were identified by Fourier transform infrared spectral analysis. Thermal behaviour and stability of NTF were studied by thermogravimetric and differential thermal analysis and differential scanning calorimetry. Mechanical and dielectric properties of NTF crystals were analyzed. Optical studies reveal that NTF crystals are transparent in the wavelength range 286-1100 nm. The third order nonlinear optical parameters of NTF were derived by the Z-scan technique.

  6. Phase retrieval of diffraction from highly strained crystals

    International Nuclear Information System (INIS)

    Newton, Marcus C.; Harder, Ross; Huang Xiaojing; Xiong Gang; Robinson, Ian K.

    2010-01-01

    An important application of phase retrieval methods is to invert coherent x-ray diffraction measurements to obtain real-space images of nanoscale crystals. The phase information is currently recovered from reciprocal-space amplitude measurements by the application of iterative projective algorithms that solve the nonlinear and nonconvex optimization problem. Various algorithms have been developed each of which apply constraints in real and reciprocal space on the reconstructed object. In general, these methods rely on experimental data that is oversampled above the Nyquist frequency. To date, support-based methods have worked well, but are less successful for highly strained structures, defined as those which contain (real-space) phase information outside the range of ±π/2. As a direct result the acquired experimental data is, in general, inadvertently subsampled below the Nyquist frequency. In recent years, a new theory of 'compressive sensing' has emerged, which dictates that an appropriately subsampled (or compressed) signal can be recovered exactly through iterative reconstruction and various routes to minimizing the l 1 norm or total variation in that signal. This has proven effective in solving several classes of convex optimization problems. Here we report on a 'density-modification' phase reconstruction algorithm that applies the principles of compressive sensing to solve the nonconvex phase retrieval problem for highly strained crystalline materials. The application of a nonlinear operator in real-space minimizes the l 1 norm of the amplitude by a promotion-penalization (or 'propenal') operation that confines the density bandwidth. This was found to significantly aid in the reconstruction of highly strained nanocrystals. We show how this method is able to successfully reconstruct phase information that otherwise could not be recovered.

  7. Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.; Hunt, D.; Hahn, D.; Cradick, J. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Morgan, D. V. [National Security Technologies LLC, Los Alamos, New Mexico 87544 (United States)

    2016-08-15

    Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from the sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.

  8. Growth, structural, optical and surface analysis of piperazinium tartrate: A NLO single crystal

    Science.gov (United States)

    Gupta, Apurva; Raseel Rahman M., K.; Nair, Lekha

    2018-05-01

    Single crystal of piperazinium tartrate (PPZT) was grown by the slow evaporation solution growth technique at room temperature. Crystallinity of grown crystal was examined by powder X-ray diffraction. High transparency and wide band gap were observed in the UV-Visible spectroscopic studies. Intense and broad emissions were observed in the blue region, as that is indicated by photoluminescence spectroscopy. The quality of the grown PPZT single crystals were analyzed by the etching studies using the water as the etchant.

  9. Electrically Anisotropic Layered Perovskite Single Crystal

    KAUST Repository

    Li, Ting-You

    2016-04-01

    Organic-inorganic hybrid perovskites (OIHPs), which are promising materials for electronic and optoelectronic applications (1-10), have made into layered organic-inorganic hybrid perovskites (LOIHPs). These LOIHPs have been applied to thin-film transistors, solar cells and tunable wavelength phosphors (11-18). It is known that devices fabricated with single crystal exhibit the superior performance, which makes the growth of large-sized single crystals critical for future device applications (19-23). However, the difficulty in growing large-sized LOIHPs single crystal with superior electrical properties limits their practical applications. Here, we report a method to grow the centimeter-scaled LOIHP single crystal of [(HOC2H4NH3)2PbI4], demonstrating the potentials in mass production. After that, we reveal anisotropic electrical and optoelectronic properties which proved the carrier propagating along inorganic framework. The carrier mobility of in-inorganic-plane (in-plane) devices shows the average value of 45 cm2 V–1 s–1 which is about 100 times greater than the record of LOIHP devices (15), showing the importance of single crystal in device application. Moreover, the LOIHP single crystals show its ultra-short carrier lifetime of 42.7 ps and photoluminescence quantum efficiency (PLQE) of 25.4 %. We expect this report to be a start of LOIHPs for advanced applications in which the anisotropic properties are needed (24-25), and meets the demand of high-speed applications and fast-response applications.

  10. Single Crystals Grown Under Unconstrained Conditions

    Science.gov (United States)

    Sunagawa, Ichiro

    Based on detailed investigations on morphology (evolution and variation in external forms), surface microtopography of crystal faces (spirals and etch figures), internal morphology (growth sectors, growth banding and associated impurity partitioning) and perfection (dislocations and other lattice defects) in single crystals, we can deduce how and by what mechanism the crystal grew and experienced fluctuation in growth parameters through its growth and post-growth history under unconstrained condition. The information is useful not only in finding appropriate way to growing highly perfect and homogeneous single crystals, but also in deciphering letters sent from the depth of the Earth and the Space. It is also useful in discriminating synthetic from natural gemstones. In this chapter, available methods to obtain molecular information are briefly summarized, and actual examples to demonstrate the importance of this type of investigations are selected from both natural minerals (diamond, quartz, hematite, corundum, beryl, phlogopite) and synthetic crystals (SiC, diamond, corundum, beryl).

  11. Structural and optical properties of WTe2 single crystals synthesized by DVT technique

    Science.gov (United States)

    Dixit, Vijay; Vyas, Chirag; Pathak, V. M.; Soalanki, G. K.; Patel, K. D.

    2018-05-01

    Layered transition metal di-chalcogenide (LTMDCs) crystals have attracted much attention due to their potential in optoelectronic device applications recently due to realization of their monolayer based structures. In the present investigation we report growth of WTe2 single crystals by direct vapor transport (DVT) technique. These crystals are then characterized by energy dispersive analysis of x-rays (EDAX) to study stoichiometric composition after growth. The structural properties are studied by x-ray diffraction (XRD) and selected area electron diffraction (SAED) is used to confirm orthorhombic structure of grown WTe2 crystal. Surface morphological properties of the crystals are also studied by scanning electron microscope (SEM). The optical properties of the grown crystals are studied by UV-Visible spectroscopy which gives direct band gap of 1.44 eV for grown WTe2 single crystals.

  12. Crystallization and preliminary X-ray diffraction analysis of the lytic transglycosylase MltE from Escherichia coli

    International Nuclear Information System (INIS)

    Artola-Recolons, Cecilia; Llarrull, Leticia I.; Lastochkin, Elena; Mobashery, Shahriar; Hermoso, Juan A.

    2010-01-01

    Crystals of the lytic transglycosylase MltE from E. coli were grown using the microbatch method and diffracted to a resolution of 2.1 Å. MltE from Escherichia coli (193 amino acids, 21 380 Da) is a lytic transglycosylase that initiates the first step of cell-wall recycling. This enzyme is responsible for the cleavage of the cell-wall peptidoglycan at the β-1,4-glycosidic bond between the N-acetylglucosamine and N-acetylmuramic acid units. At the end this reaction generates a disaccharide that is internalized and initiates the recycling process. To obtain insights into the biological functions of MltE, crystallization trials were performed and crystals of MltE protein that were suitable for X-ray diffraction analysis were obtained. The MltE protein of E. coli was crystallized using the hanging-drop vapour-diffusion method at 291 K. Crystals grew from a mixture consisting of 28% polyethylene glycol 4000, 0.1 M Tris pH 8.4 and 0.2 M magnesium chloride. Further optimization was performed using the microbatch technique. Single crystals were obtained that belonged to the orthorhombic space group C222 1 , with unit-cell parameters a = 123.32, b = 183.93, c = 35.29 Å, and diffracted to a resolution of 2.1 Å

  13. Crystallization and preliminary X-ray diffraction analysis of a specific VHH domain against mouse prion protein

    International Nuclear Information System (INIS)

    Abskharon, Romany N. N.; Soror, Sameh H.; Pardon, Els; El Hassan, Hassan; Legname, Giuseppe; Steyaert, Jan; Wohlkonig, Alexandre

    2010-01-01

    The crystallization of a specific nanobody against mouse PrP C and preliminary diffraction analysis of a crystal that diffracted to 1.23 Å resolution are presented. Prion disorders are infectious diseases that are characterized by the conversion of the cellular prion protein PrP C into the pathogenic isoform PrP Sc . Specific antibodies that interact with the cellular prion protein have been shown to inhibit this transition. Recombinant VHHs (variable domain of dromedary heavy-chain antibodies) or nanobodies are single-domain antibodies, making them the smallest antigen-binding fragments. A specific nanobody (Nb-PrP-01) was raised against mouse PrP C . A crystallization condition for this recombinant nanobody was identified using high-throughput screening. The crystals were optimized using streak-seeding and the hanging-drop method. The crystals belonged to the orthorhombic space group P2 1 2 1 2 1 , with unit-cell parameters a = 30.04, b = 37.15, c = 83.00 Å, and diffracted to 1.23 Å resolution using synchrotron radiation. The crystal structure of this specific nanobody against PrP C together with the known PrP C structure may help in understanding the PrP C /PrP Sc transition mechanism

  14. Purification, crystallization and preliminary X-ray diffraction studies of parakeet (Psittacula krameri) haemoglobin.

    Science.gov (United States)

    Jaimohan, S M; Naresh, M D; Arumugam, V; Mandal, A B

    2009-10-01

    Birds often show efficient oxygen management in order to meet the special demands of their metabolism. However, the structural studies of avian haemoglobins (Hbs) are inadequate for complete understanding of the mechanism involved. Towards this end, purification, crystallization and preliminary X-ray diffraction studies have been carried out for parakeet Hb. Parakeet Hb was crystallized as the met form in low-salt buffered conditions after extracting haemoglobin from crude blood by microcentrifugation and purifying the sample by column chromatography. Good-quality crystals were grown from 10% PEG 3350 and a crystal diffracted to about 2.8 A resolution. Preliminary diffraction data showed that the Hb crystal belonged to the monoclinic system (space group C2), with unit-cell parameters a = 110.68, b = 64.27, c = 56.40 A, beta = 109.35 degrees . Matthews volume analysis indicated that the crystals contained a half-tetramer in the asymmetric unit.

  15. Effect of Metal Dopant on Ninhydrin—Organic Nonlinear Optical Single Crystals

    Directory of Open Access Journals (Sweden)

    R. S. Sreenivasan

    2013-01-01

    Full Text Available In the present work, metal (Cu2+-substituted ninhydrin single crystals were grown by slow evaporation method. The grown crystals have been subjected to single crystal XRD, powder X-ray diffraction, FTIR, dielectric and SHG studies. Single crystal X-ray diffraction analysis reveals that the compound crystallizes in monoclinic system with noncentrosymmetric space group P21 with lattice parameters a=11.28 Å, b=5.98 Å, c=5.71 Å, α=90∘, β=98.57, γ=90∘, and V=381 (Å3, which agrees very well with the reported value. The sharp and strong peaks in the powder X-ray diffraction pattern confirm the good crystallinity of the grown crystals. The presence of dopants marginally altered the lattice parameters without affecting the basic structure of the crystal. The UV-Vis transmittance spectrum shows that the crystal has a good optical transmittance in the entire visible region with lower cutoff wavelength 314 nm. The vibrational frequencies of various functional groups in the crystals have been derived from FT-IR analysis. Based on the shifts in the vibrations, the presence of copper in the lattice of the grown crystal is clearly established from the pure ninhydrin crystals. Both dielectric constant and dielectric loss decrease with the increase in frequency. The second harmonic generation efficiency was measured by employing powder Kurtz method.

  16. Correct interpretation of diffraction properties of quartz crystals for X-ray optics applications

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Xian-Rong; Gog, Thomas; Kim, Jungho; Kasman, Elina; Said, Ayman H.; Casa, Diego M.; Wieczorek, Michael; Hönnicke, Marcelo G.; Assoufid, Lahsen

    2018-02-01

    Quartz has hundreds of strong Bragg reflections that may offer a great number of choices for making fixed-angle X-ray analyzers and polarizers at virtually any hard X-ray energies with selectable resolution. However, quartz crystals, unlike silicon and germanium, are chiral and may thus appear in two different forms of handedness that are mirror images. Furthermore, because of the threefold rotational symmetry along thecaxis, the {h1h2h3L} and {h2h1h3L} Bragg reflections may have quite different Darwin bandwidth, reflectivity and angular acceptance, although they have the same Bragg angle. The design of X-ray optics from quartz crystals therefore requires unambiguous determination of the orientation, handedness and polarity of the crystals. The Laue method and single-axis diffraction technique can provide such information, but the variety of conventions used in the literature to describe quartz structures has caused widespread confusion. The current studies give detailed guidelines for design and fabrication of quartz X-ray optics, with special emphasis on the correct interpretation of Laue patterns in terms of the crystallography and diffraction properties of quartz. Meanwhile, the quartz crystals examined were confirmed by X-ray topography to have acceptably low densities of dislocations and other defects, which is the foundation for developing high-resolution quartz-based X-ray optics.

  17. A universal treatment of X-ray and neutron diffraction in crystals. II. Extinction

    International Nuclear Information System (INIS)

    Hu Huachen

    1997-01-01

    For pt.I see ibid., p.484-92, 1997. Based on the formalism for calculating the integrated reflection power ratio of a plane mosaic crystal by using three dimensionless parameters exact and universal expressions for the secondary-extinction factors in X-ray and neutron crystallography are developed that can be applied to reflections of all possible values of extinction factor, reflection symmetry and the absorption-to-scattering cross-section ratio of the crystal. The representation by three parameters gives a clear and definite physical meaning to the concept of extinction. The theory has been extended to treat the extinction of a spherical crystal, and the striking difference in the evaluated secondary-extinction factor between the equivalent single-plate and the exact method in the spherical-crystal treatment under θ B = 0 is explained. As a demonstration of the feasibility of using these expressions, the diffraction data for LiF and MgO crystal plates measured by Lawrence [Acta Cryst. (1972), A28, 400-404; (1973), A29, 208-210] are reanalyzed by this method. All the reflections including the strongest ones (Y o down to 0.026) are reanalyzed simultaneously with single-valued particle size and mosaic spread as fitting parameters and allowing for primary extinction if necessary. The results (R factor = 0.014 and 0.053 for LiF and MgO, respectively) are unprecedentedly good. Furthermore, in disagreement with Lawrence, the extinction of LiF is found to be of secondary type and in the case of MgO both primary and secondary extinction should be considered. The analysis also shows that the formula Y ∝ Y p Y s is valid only for very weak extinctions and that the Hamilton-Darwin equations are valid in a range much broader than previously anticipated. (orig.)

  18. Syntheses and crystal structure determination by X-ray powder diffraction of new compounds of Benzovesamicol

    International Nuclear Information System (INIS)

    Rukiah, M.; Assaad, Th.

    2012-06-01

    The compound 2,2,2-Trifluoro-N-(1a,2,7,7 a-tetra-hydronaphtho[2,3-b]oxiren-3-yl)- acetamide, C 1 2H 1 0F 3 NO 2 , an important precursor in the preparation of benzovesamicol analogues for the diagnosis of Alzheimers disease, was prepared by the epoxidation of 5,8-dihydronaphthalene-1-amine using 3-chloroperoxybenzoic acid. The structure was determined by X-ray powder diffraction, multinuclear NMR spectroscopy and FT-IR spectroscopy. A pair of molecules form intermolecular N- H...O hydrogen bonds, involving the amino and oxirene groups, to produce a dimer.The two racemic compounds (2RS,3RS)-5-amino-3-(4-phenylpiperazin-1-yl)-1,2,3,4 tetrahydronaphthalene-2-ol, C 2 0H 2 5N 3 O, (I) and (2RS,3RS)-5-amino-3-[4-(3- methoxyphenyl)piperazin-1-yl]-1,2,3,4-tetrahydronaphthalene-2-ol, C 2 1H 2 7N 3 O 2 , (II) important benzovesamicol analogues for the diagnosis of Alzheimer's disease, have been synthesized and characterized by FT-IR, and 1 H and 13 C NMR spectroscopic analyses. The crystal structures were analyses using powder diffraction as no suitable single crystal were obtained. The two compounds are racemic mixtures of enantiomers which crystallize in the monoclinic system in a centrosymmetric space group (P21/c). Crystallography, in particular powder X-ray diffraction, was pivotal in revealing that the enantio-resolution did not succeed. In two compounds, the piperazine ring has a chair conformation, while the cyclohexene ring assumes a half-chair conformation. In (I) the crystal packing is mediated by weak contacts, principally by complementary intermolecular N--H...O hydrogen bonds that connect successive molecules into a chain. Further stabilization is provided by weak C--H...N contacts and by a weak intermolecular C--H...π interaction. While in (II), the crystal packing is dominated by intermolecular O--H...N hydrogen bonding which links molecules along the c direction. (authors)

  19. Crystal plasticity study of single crystal tungsten by indentation tests

    International Nuclear Information System (INIS)

    Yao, Weizhi

    2012-01-01

    Owing to its favorable material properties, tungsten (W) has been studied as a plasma-facing material in fusion reactors. Experiments on W heating in plasma sources and electron beam facilities have shown an intense micro-crack formation at the heated surface and sub-surface. The cracks go deep inside the irradiated sample, and often large distorted areas caused by local plastic deformation are present around the cracks. To interpret the crack-induced microscopic damage evolution process in W, one needs firstly to understand its plasticity on a single grain level, which is referred to as crystal plasticity. In this thesis, the crystal plasticity of single crystal tungsten (SCW) has been studied by spherical and Berkovich indentation tests and the finite element method with a crystal plasticity model. Appropriate values of the material parameters included in the crystal plasticity model are determined by fitting measured load-displacement curves and pile-up profiles with simulated counterparts for spherical indentation. The numerical simulations reveal excellent agreement with experiment. While the load-displacement curves and the deduced indentation hardness exhibit little sensitivity to the indented plane at small indentation depths, the orientation of slip directions within the crystals governs the development of deformation hillocks at the surface. It is found that several factors like friction, indentation depth, active slip systems, misoriented crystal orientation, misoriented sample surface and azimuthal orientation of the indenter can affect the indentation behavior of SCW. The Berkovich indentation test was also used to study the crystal plasticity of SCW after deuterium irradiation. The critical load (pop-in load) for triggering plastic deformation under the indenter is found to depend on the crystallographic orientation. The pop-in loads decrease dramatically after deuterium plasma irradiation for all three investigated crystallographic planes.

  20. Crystallization and preliminary X-ray diffraction analysis of West Nile virus

    International Nuclear Information System (INIS)

    Kaufmann, Bärbel; Plevka, Pavel; Kuhn, Richard J.; Rossmann, Michael G.

    2010-01-01

    Crystals of infectious West Nile virus were obtained and diffracted at best to about 25 Å resolution. Preliminary analysis of the diffraction pattern suggested tight hexagonal packing of the intact virus. West Nile virus, a human pathogen, is closely related to other medically important flaviviruses of global impact such as dengue virus. The infectious virus was purified from cell culture using polyethylene glycol (PEG) precipitation and density-gradient centrifugation. Thin amorphously shaped crystals of the lipid-enveloped virus were grown in quartz capillaries equilibrated by vapor diffusion. Crystal diffraction extended at best to a resolution of about 25 Å using synchrotron radiation. A preliminary analysis of the diffraction images indicated that the crystals had unit-cell parameters a ≃ b ≃ 480 Å, γ = 120°, suggesting a tight hexagonal packing of one virus particle per unit cell

  1. Single shot diffraction of picosecond 8.7-keV x-ray pulses

    Directory of Open Access Journals (Sweden)

    F. H. O’Shea

    2012-02-01

    Full Text Available We demonstrate multiphoton, single shot diffraction images of x rays produced by inverse Compton scattering a high-power CO_{2} laser from a relativistic electron beam, creating a pulse of 8.7 keV x rays. The tightly focused, relatively high peak brightness electron beam and high photon density from the 2 J CO_{2} laser yielded 6×10^{7} x-ray photons over the full opening angle in a single shot. Single shot x-ray diffraction is performed by passing the x rays though a vertical slit and on to a flat silicon (111 crystal. 10^{2} diffracted photons were detected. The spectrum of the detected x rays is compared to simulation. The diffraction and detection of 10^{2} x rays is a key step to a more efficient time resolved diagnostic in which the number of observed x rays might reach 10^{4}; enabling a unique, flexible x-ray source as a sub-ps resolution diagnostic for studying the evolution of chemical reactions, lattice deformation and melting, and magnetism.

  2. Single Crystal Diffuse Neutron Scattering

    Directory of Open Access Journals (Sweden)

    Richard Welberry

    2018-01-01

    Full Text Available Diffuse neutron scattering has become a valuable tool for investigating local structure in materials ranging from organic molecular crystals containing only light atoms to piezo-ceramics that frequently contain heavy elements. Although neutron sources will never be able to compete with X-rays in terms of the available flux the special properties of neutrons, viz. the ability to explore inelastic scattering events, the fact that scattering lengths do not vary systematically with atomic number and their ability to scatter from magnetic moments, provides strong motivation for developing neutron diffuse scattering methods. In this paper, we compare three different instruments that have been used by us to collect neutron diffuse scattering data. Two of these are on a spallation source and one on a reactor source.

  3. A structural study of [CpM(CO)3H] (M = Cr, Mo and W) by single-crystal X-ray diffraction and DFT calculations: sterically crowded yet surprisingly flexible molecules.

    Science.gov (United States)

    Burchell, Richard P L; Sirsch, Peter; Decken, Andreas; McGrady, G Sean

    2009-08-14

    The single-crystal X-ray structures of the complexes [CpCr(CO)3H] 1, [CpMo(CO)3H] 2 and [CpW(CO)3H] 3 are reported. The results indicate that 1 adopts a structure close to a distorted three-legged piano stool geometry, whereas a conventional four-legged piano stool arrangement is observed for 2 and 3. Further insight into the equilibrium geometries and potential energy surfaces of all three complexes was obtained by DFT calculations. These show that in the gas phase complex 1 also prefers a geometry close to a four-legged piano stool in line with its heavier congeners, and implying strong packing forces at work for 1 in the solid state. Comparison with their isolelectronic group 7 tricarbonyl counterparts [CpM(CO)3] (M = Mn 4 and Re 5) illustrates that 1, 2 and 3 are sterically crowded complexes. However, a surprisingly soft bending potential is evident for the M-H moiety, whose order (1 approximately = 2 < 3) correlates with the M-H bond strength rather than with the degree of congestion at the metal centre, indicating electronic rather than steric control of the potential. The calculations also reveal cooperative motions of the hydride and carbonyl ligands in the M(CO)3H unit, which allow the M-H moiety to move freely, in spite of the closeness of the four basal ligands, helping to explain the surprising flexibility of the crowded coordination sphere observed for this family of high CN complexes.

  4. Bloch walls in a nickel single crystal

    International Nuclear Information System (INIS)

    Peters, J.; Treimer, W.

    2001-01-01

    We present a consistent theory for the dependence of the magnetic structure in bulk samples on external static magnetic fields and corresponding experimental results. We applied the theory of micromagnetism to this crystal and calculated the Bloch wall thickness as a function of external magnetic fields. The theoretical results agree well with the experimental data, so that the Bloch wall thickness of a 71 deg. nickel single crystal was definitely determined with some hundred of nanometer

  5. Synthesis, crystal growth, optical, thermal, and mechanical properties of a nonlinear optical single crystal: ammonium sulfate hydrogen sulphamate (ASHS)

    Science.gov (United States)

    Sudhakar, K.; Nandhini, S.; Muniyappan, S.; Arumanayagam, T.; Vivek, P.; Murugakoothan, P.

    2018-04-01

    Ammonium sulfate hydrogen sulphamate (ASHS), an inorganic nonlinear optical crystal, was grown from the aqueous solution by slow evaporation solution growth technique. The single-crystal XRD confirms that the grown single crystal belongs to the orthorhombic system with the space group of Pna21. Powder XRD confirms the crystalline nature and the diffraction planes were indexed. Crystalline perfection of grown crystal was analysed by high-resolution X-ray diffraction rocking curve technique. UV-Vis-NIR studies revealed that ASHS crystal has optical transparency 65% and lower cut-off wavelength at 218 nm. The violet light emission of the crystal was identified by photoluminescence studies. The particle size-dependent second-harmonic generation efficiency for ASHS crystal was evaluated by Kurtz-Perry powder technique using Nd:YAG laser which established the existence of phase matching. Surface laser damage threshold value was evaluated using Nd:YAG laser. Optical homogeneity of the crystal was evaluated using modified channel spectrum method through birefringence study. Thermal analysis reveals that ASHS crystal is stable up to 213 °C. The mechanical behaviour of the ASHS crystal was analysed using Vickers microhardness study.

  6. Improving the diffraction of apoA-IV crystals through extreme dehydration

    International Nuclear Information System (INIS)

    Deng, Xiaodi; Davidson, W. Sean; Thompson, Thomas B.

    2011-01-01

    Apolipoprotein A-IV crystals consisted of a long unit-cell edge (540 Å) with a high mosaic spread, making them intractable for X-ray diffraction analysis. Extreme dehydration in 60% PEG 3350 was utilized as a post-crystallization treatment as well a screening method to significantly sharpen the mosaic spread and increase the overall resolution of diffraction. Apolipoproteins are the protein component of high-density lipoproteins (HDL), which are necessary for mobilizing lipid-like molecules throughout the body. Apolipoproteins undergo self-association, especially at higher concentrations, making them difficult to crystallize. Here, the crystallization and diffraction of the core fragment of apolipoprotein A-IV (apoA-IV), consisting of residues 64–335, is presented. ApoA-IV 64–335 crystallized readily in a variety of hexagonal (P6) morphologies with similar unit-cell parameters, all containing a long axis of nearly 550 Å in length. Preliminary diffraction experiments with the different crystal morphologies all resulted in limited streaky diffraction to 3.5 Å resolution. Crystal dehydration was applied to the different morphologies with variable success and was also used as a quality indicator of crystal-growth conditions. The results show that the morphologies that withstood the most extreme dehydration conditions showed the greatest improvement in diffraction. One morphology in particular was able to withstand dehydration in 60% PEG 3350 for over 12 h, which resulted in well defined intensities to 2.7 Å resolution. These results suggest that the approach of integrating dehydration with variation in crystal-growth conditions might be a general technique to optimize diffraction

  7. Aluminum-rich mesoporous MFI - type zeolite single crystals

    DEFF Research Database (Denmark)

    Kustova, Marina; Kustov, Arkadii; Christensen, Christina Hviid

    2005-01-01

    Zeolitcs are crystalline materials, which are widely used as solid acid catalysts and supports in many industrial processes. Recently, mesoporous MFI-type zeolite single crystals were synthesized by use of carbon particles as a mesopore template and sodium aluminate as the aluminum Source....... With this technique, only zeolites with relatively low Al contents were reported (Si/Al ratio about 100). In this work, the preparation of aluminum-rich mesoporous MFI-type zeolite single crystals (Si/Al similar to 16-50) using aluminum isopropoxide as the aluminum Source is reported for the first time. All samples...... are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), ammonia temperature programmed desorption (NH3-TPD), and N-2 adsorption measurements. The obtained zeolites combine the high crystallinity and the characteristic micropores of zeolites with an intracrystalline mesopore system...

  8. Blazed vector gratings fabricated using photosensitive polymer liquid crystals and control of polarization diffraction

    Science.gov (United States)

    Ono, Hiroshi; Kuzuwata, Mitsuru; Sasaki, Tomoyuki; Noda, Kohei; Kawatsuki, Nobuhiro

    2014-03-01

    The blazed vector grating possessing antisymmetric distributions of the birefringence were fabricated by exposing the line-focused linearly polarized ultraviolet light on the photosensitive polymer liquid crystals. The polarization states of the diffraction beams can be highly and widely controlled by designing the blazed structures, and the diffraction properties were well-explained by Jones calculus.

  9. Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation.

    Science.gov (United States)

    Hrdý, Jaromír; Mikulík, Petr; Oberta, Peter

    2011-03-01

    A new kind of two channel-cut crystals X-ray monochromator in dispersive (+,-,-,+) position which spatially separates harmonics is proposed. The diffracting surfaces are oriented so that the diffraction is inclined. Owing to refraction the diffracted beam is sagittally deviated. The deviation depends on wavelength and is much higher for the first harmonics than for higher harmonics. This leads to spatial harmonics separation. The idea is supported by ray-tracing simulation.

  10. Quantitative reconstruction from a single diffraction-enhanced image

    International Nuclear Information System (INIS)

    Paganin, D.M.; Lewis, R.A.; Kitchen, M.

    2003-01-01

    Full text: We develop an algorithm for using a single diffraction-enhanced image (DEI) to obtain a quantitative reconstruction of the projected thickness of a single-material sample which is embedded within a substrate of approximately constant thickness. This algorithm is used to quantitatively map inclusions in a breast phantom, from a single synchrotron DEI image. In particular, the reconstructed images quantitatively represent the projected thickness in the bulk of the sample, in contrast to DEI images which greatly emphasise sharp edges (high spatial frequencies). In the context of an ultimate aim of improved methods for breast cancer detection, the reconstructions are potentially of greater diagnostic value compared to the DEI data. Lastly, we point out that the methods of analysis presented here are also applicable to the quantitative analysis of differential interference contrast (DIC) images

  11. Electronic transport properties of single crystal thallium-2201 superconductors

    International Nuclear Information System (INIS)

    Yandrofski, R.M.

    1992-01-01

    Four-probe resistance measurements on single crystals of the calcium-free thallium-based superconducting Tl 2 Ba 2 CuO 6+σ phase (Tl-2201) were performed in magnetic fields up to 12 Telsa. Single crystals of sizes were grown by a self-flux technique and were characterized by single crystal X-ray diffraction and X-ray Dispersive Analysis. Field measurements were taken at dc and at low frequencies using a lock-in technique. Techniques were developed to oxygen-anneal the as-grown single crystals to generate single crystal samples of the same Tl-2201 phase with varying transition interaction effect against appropriate composite general alternatives are developed for the standard two-way layout with a single observation per cell. Nonparametric aligned-rank test procedures are introduced. One of the new procedures is shown to be equivalent to a slight modification of the previously studied Latin square procedures when the factors have the same number of levels. The equal in distribution technique is used to show that any statistic based on the joint ranks should not be used to test the hypotheses of interest. The tests based on aligning with the averages do not depend on the nuisance main effects, while those based on aligning with the median do depend on the nuisance main effects. The relative power performance of the competing tests are examined via Monte Carlo simulation. Power studies conducted on the 5 x 5, 5 x 6, and 5 x 9 two-way layouts with one observation per cell show that the new procedures based on a comparison of all possible pairs of rank-profiles perform quite well for two types of product interaction, a general class of interaction effects proposed by Martin, and several sets of specific interaction effects. Approximate critical values for some of the proposed procedures are explored in the special case when the main effect parameters for one factor are known

  12. Preliminary morphological and X-ray diffraction studies of the crystals of the DNA cetyltrimethylammonium salt.

    Science.gov (United States)

    Osica, V D; Pyatigorskaya, T L; Polyvtsev, O F; Dembo, A T; Kliya, M O; Vasilchenko, V N; Verkin, B I; Sukharevskya, B Y

    1977-04-01

    Double-stranded DNA molecules (molecular weight 2.5 X 10(5) - 5 X 10(5) daltons) have been crystallized from water-salt solutions as cetyltrimethylammonium salts (CTA-DNA). Variation of crystallization conditions results in a production of different types of CTA-DNA crystals: spherulits, dendrites, needle-shaped and faceted rhombic crystals, the latter beeing up to 0.3 mm on a side. X-ray diffraction data indicate that DNA molecules in the crystals form a hexagonal lattice which parameters vary slightly with the morphological type of the crystal. Comparison of the melting curves of the DNA preparation before and after crystallization suggests that DNA molecules are partially fractionated in the course of crystallization. Crystals of the CTA-DNA-proflavine complex have also been obtained.

  13. Parametric X-rays and diffracted transition radiation in perfect and mosaic crystals

    International Nuclear Information System (INIS)

    Artru, X.; Rullhusen, P.

    1998-01-01

    The amplitude of X-ray emission by relativistic electrons in a single crystal, calculated in the kinematical approach, is decomposed unambiguously in Diffracted Transition Radiation (DTR) and Parametric X-rays (PXR). DTR becomes significant for γ > or similar to ω P ,γ being the Lorentz factor and ω P the plasma frequency. It is more collimated than PXR and, above threshold, its flux increases logarithmically with γ. However, it saturates with thickness at the Bragg primary extinction length l e . This saturation is accounted for only in the dynamical approach, the formulas of which are compared to the kinematical ones. The respective contributions of DTR and PXR are calculated for a simple model of mosaic crystal, taking into account saturation of DTR with thickness. The PXR flux is basically the same as in a perfect crystal. If the size of the domains is larger than l e , the DTR flux is multiplied by the number of domains crossed by the electron. For domains smaller than l e and γ > or similar to ω P , the DTR and PXR fluxes are of the same order of magnitude, up to logarithmic factors. In any case, mosaicity increases the total yield of X-ray photons. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Haugh, M. J., E-mail: haughmj@nv.doe.gov; Jacoby, K. D. [National Security Technologies, LLC, Livermore, California 94550 (United States); Wu, M.; Loisel, G. P. [Sandia National Laboratories, Albuquerque, New Mexico 87123 (United States)

    2014-11-15

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

  16. X-CHIP: an integrated platform for high-throughput protein crystallization and on-the-chip X-ray diffraction data collection

    International Nuclear Information System (INIS)

    Kisselman, Gera; Qiu, Wei; Romanov, Vladimir; Thompson, Christine M.; Lam, Robert; Battaile, Kevin P.; Pai, Emil F.; Chirgadze, Nickolay Y.

    2011-01-01

    The X-CHIP (X-ray Crystallography High-throughput Integrated Platform) is a novel microchip that has been developed to combine multiple steps of the crystallographic pipeline from crystallization to diffraction data collection on a single device to streamline the entire process. The X-CHIP (X-ray Crystallization High-throughput Integrated Platform) is a novel microchip that has been developed to combine multiple steps of the crystallographic pipeline from crystallization to diffraction data collection on a single device to streamline the entire process. The system has been designed for crystallization condition screening, visual crystal inspection, initial X-ray screening and data collection in a high-throughput fashion. X-ray diffraction data acquisition can be performed directly on-the-chip at room temperature using an in situ approach. The capabilities of the chip eliminate the necessity for manual crystal handling and cryoprotection of crystal samples, while allowing data collection from multiple crystals in the same drop. This technology would be especially beneficial for projects with large volumes of data, such as protein-complex studies and fragment-based screening. The platform employs hydrophilic and hydrophobic concentric ring surfaces on a miniature plate transparent to visible light and X-rays to create a well defined and stable microbatch crystallization environment. The results of crystallization and data-collection experiments demonstrate that high-quality well diffracting crystals can be grown and high-resolution diffraction data sets can be collected using this technology. Furthermore, the quality of a single-wavelength anomalous dispersion data set collected with the X-CHIP at room temperature was sufficient to generate interpretable electron-density maps. This technology is highly resource-efficient owing to the use of nanolitre-scale drop volumes. It does not require any modification for most in-house and synchrotron beamline systems and offers

  17. X-CHIP: an integrated platform for high-throughput protein crystallization and on-the-chip X-ray diffraction data collection

    Energy Technology Data Exchange (ETDEWEB)

    Kisselman, Gera; Qiu, Wei; Romanov, Vladimir; Thompson, Christine M.; Lam, Robert [Ontario Cancer Institute, Princess Margaret Hospital, University Health Network, Toronto, Ontario M5G 2C4 (Canada); Battaile, Kevin P. [Argonne National Laboratory, Argonne, Illinois 60439 (United States); Pai, Emil F.; Chirgadze, Nickolay Y., E-mail: nchirgad@uhnresearch.ca [Ontario Cancer Institute, Princess Margaret Hospital, University Health Network, Toronto, Ontario M5G 2C4 (Canada); University of Toronto, Toronto, Ontario M5S 1A8 (Canada)

    2011-06-01

    The X-CHIP (X-ray Crystallography High-throughput Integrated Platform) is a novel microchip that has been developed to combine multiple steps of the crystallographic pipeline from crystallization to diffraction data collection on a single device to streamline the entire process. The X-CHIP (X-ray Crystallization High-throughput Integrated Platform) is a novel microchip that has been developed to combine multiple steps of the crystallographic pipeline from crystallization to diffraction data collection on a single device to streamline the entire process. The system has been designed for crystallization condition screening, visual crystal inspection, initial X-ray screening and data collection in a high-throughput fashion. X-ray diffraction data acquisition can be performed directly on-the-chip at room temperature using an in situ approach. The capabilities of the chip eliminate the necessity for manual crystal handling and cryoprotection of crystal samples, while allowing data collection from multiple crystals in the same drop. This technology would be especially beneficial for projects with large volumes of data, such as protein-complex studies and fragment-based screening. The platform employs hydrophilic and hydrophobic concentric ring surfaces on a miniature plate transparent to visible light and X-rays to create a well defined and stable microbatch crystallization environment. The results of crystallization and data-collection experiments demonstrate that high-quality well diffracting crystals can be grown and high-resolution diffraction data sets can be collected using this technology. Furthermore, the quality of a single-wavelength anomalous dispersion data set collected with the X-CHIP at room temperature was sufficient to generate interpretable electron-density maps. This technology is highly resource-efficient owing to the use of nanolitre-scale drop volumes. It does not require any modification for most in-house and synchrotron beamline systems and offers

  18. Hard single diffractive jet production at D0

    International Nuclear Information System (INIS)

    Abachi, S.; Abbott, B.; Abolins, M.

    1996-08-01

    Preliminary results from the D null experiment on jet production with forward rapidity gaps in p anti p collisions are presented. A class of dijet events with a forward rapidity gap is observed at center-of-mass energies √s = 1800 GeV and 630 GeV. The number of events with rapidity gaps at both center-of-mass energies is significantly greater than the expectation from multiplicity fluctuations and is consistent with a hard single diffractive process. A small class of events with two forward gaps and central dijets is also observed at 1800 GeV. This topology is consistent with hard double pomeron exchange

  19. Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto

    OpenAIRE

    Yanagisawa, Yasuhide; Chatake, Toshiyuki; Chiba-Kamoshida, Kaori; Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki; Yasuda, Ichiro; Morimoto, Yukio

    2010-01-01

    Nattokinase, a protein found in high levels in the traditional Japanese food natto, has been reported to have high thrombolytic activity. In the present study, the crystallization of native nattokinase and the collection of X-ray diffraction date from a nattokinase crystal to a resolution of 1.74 Å are reported.

  20. Plastic deformation of submicron-sized crystals studied by in-situ Kikuchi diffraction and dislocation imaging

    DEFF Research Database (Denmark)

    Zhang, Xiaodan; Godfrey, Andrew; Winther, Grethe

    2012-01-01

    The plastic deformation of submicron-size copper single crystals in the form of pillars has been characterized during in-situ compression in the transmission electron microscope up to strains of 28–33% using a state-of-the-art holder (PI-95 PicoIndenter). The dimensions of the crystals used were...... approx. 500×250×200 nm3 with the compression axis oriented 1.6° from [110]. Local crystallographic orientations have been determined with high accuracy using a Kikuchi diffraction method and glide of dislocations over a pillar has also been observed directly by dark field imaging. The variation...

  1. Inkjet printing of single-crystal films.

    Science.gov (United States)

    Minemawari, Hiromi; Yamada, Toshikazu; Matsui, Hiroyuki; Tsutsumi, Jun'ya; Haas, Simon; Chiba, Ryosuke; Kumai, Reiji; Hasegawa, Tatsuo

    2011-07-13

    The use of single crystals has been fundamental to the development of semiconductor microelectronics and solid-state science. Whether based on inorganic or organic materials, the devices that show the highest performance rely on single-crystal interfaces, with their nearly perfect translational symmetry and exceptionally high chemical purity. Attention has recently been focused on developing simple ways of producing electronic devices by means of printing technologies. 'Printed electronics' is being explored for the manufacture of large-area and flexible electronic devices by the patterned application of functional inks containing soluble or dispersed semiconducting materials. However, because of the strong self-organizing tendency of the deposited materials, the production of semiconducting thin films of high crystallinity (indispensable for realizing high carrier mobility) may be incompatible with conventional printing processes. Here we develop a method that combines the technique of antisolvent crystallization with inkjet printing to produce organic semiconducting thin films of high crystallinity. Specifically, we show that mixing fine droplets of an antisolvent and a solution of an active semiconducting component within a confined area on an amorphous substrate can trigger the controlled formation of exceptionally uniform single-crystal or polycrystalline thin films that grow at the liquid-air interfaces. Using this approach, we have printed single crystals of the organic semiconductor 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C(8)-BTBT) (ref. 15), yielding thin-film transistors with average carrier mobilities as high as 16.4 cm(2) V(-1) s(-1). This printing technique constitutes a major step towards the use of high-performance single-crystal semiconductor devices for large-area and flexible electronics applications.

  2. Structural Characterization of Doped GaSb Single Crystals by X-ray Topography

    Energy Technology Data Exchange (ETDEWEB)

    Honnicke, M.G.; Mazzaro, I.; Manica, J.; Benine, E.; M da Costa, E.; Dedavid, B. A.; Cusatis, C.; Huang, X. R.

    2009-09-13

    We characterized GaSb single crystals containing different dopants (Al, Cd and Te), grown by the Czochralski method, by x-ray topography and high angular resolution x-ray diffraction. Lang topography revealed dislocations parallel and perpendicular to the crystal's surface. Double-crystal GaSb 333 x-ray topography shows dislocations and vertical stripes than can be associated with circular growth bands. We compared our high-angular resolution x-ray diffraction measurements (rocking curves) with the findings predicted by the dynamical theory of x-ray diffraction. These measurements show that our GaSb single crystals have a relative variation in the lattice parameter ({Delta}d/d) on the order of 10{sup -5}. This means that they can be used as electronic devices (detectors, for example) and as x-ray monochromators.

  3. Solid-melt interface structure and growth of Cu alloy single crystals

    International Nuclear Information System (INIS)

    Tomimitsu, Hiroshi; Kamada, Kohji.

    1983-01-01

    Crystal-melt interface behavior during the growth of Cu-base solid solutions by the Bridgman method is discussed on the basis of experimental evidence obtained by neutron diffraction topography. Advantages of neutron diffraction topography for the characterization of large single crystals, such as dealt with in this paper, are emphasized. Evidence was odserved of extremely regular crystal growth along directions, irrespective of the macroscopic growth direction. This contrasts with the previously believed (110) normal growth which is a conclusion of growth theory based on molecular kinetics at the solid-melt interface. In consequence, we believe that the kinetics at the interface is a minor factor in the meltgrowth of metal single crystals. Revised melt-growth theory should include both the growth and the formation of the regular structure as evidenced by neutron diffraction topography. (author)

  4. Secondary extinction in cylindrical and spherical crystals for X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Hu Huachen; Li Zhaohuan; Yang Bin; Shen Caiwan

    2001-01-01

    The distribution of the reflection power ratio for a neutron or x-ray diffracted from a cylindrical crystal immersed in an homogenous incident beam is obtained by the numerical solution of the transfer equations for the first time. The profile well reflects all the physical properties of the absorption and extinction behaviour in the crystals. A systematic investigation of the secondary extinction for cylindrical and spherical crystals was carried out based on these results

  5. The determination of the crystal structures of some uranium compounds by means of x-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Adrian, H.W.W.

    1977-10-01

    In industrial uranium processing or reprocessing procedures, aqueous uranyl nitrate solutions are an intermediate product. The compounds, whose structures are reported, might prove valuable as alternative crystallization products to existing methods of extracting the uranium from solution. The compounds are obtained by the addition of hydroxylammonium to the uranyl nitrate solution and are of the general formula UO 2 (NH 2 0) 2 .xH 2 0, where x can take the values zero, two, three and four. In addition a compound of the formula UO 2 (NH 2 0) 2 .2(NH 2 CH).2H 2 0 was obtained. The UO 2 (NH 2 0) compound crystallized in a monoclinic crystal form. Crystals large enough for neutron diffraction were not obtained. The structure of the UO 2 (NH 2 0) 2 .2H 2 0 could not be solved because only disordered crystalline material was available. The structure of UO 2 (NH 2 0) 2 .3H 2 0 was solved by means of room- and low-temperature neutron diffraction. The unit cell is orthorhombic. The structure of α-UO 2 (NH 2 0) 2 .4H 2 0 was investigated by means of room-temperature x-ray and room- and low-temperature neutron diffraction. The unit cell is triclinic. This compound strongly resembles the trihydrate. The UO 2 (NH 2 0) 2 .2(NH 2 0H).2H 2 0 compound gave crystals large enough for single crystal x-ray but not neutron diffraction. The unit cell is orthorhombic. The characteristic powder patterns (indexed except for the dihydrate compound) of the above compounds are reported [af

  6. Long wave-length x-ray diffraction crystal and method of manufacturing same

    International Nuclear Information System (INIS)

    Zingaro, W.P.; Sicignano, A.

    1980-01-01

    An x-ray diffraction crystal of the Langemuir-Blodgett type capable of detecting radiation having a wavelength greater than 50 Arystroms and a method of making such a crystal are described. The crystal consists of a pair of alternate monolayers, one a heavy metal soap, and one a light metal soap. Selecting cation pairs with a significant difference in atomic number and dispersing power, such as Pb and Be, Mg, or Ca, increases the effective interplanar distance since the Pb planes cause the predominant x-ray diffraction. (LL)

  7. Crystallization and preliminary X-ray diffraction studies of ferredoxin reductase from Leptospira interrogans

    International Nuclear Information System (INIS)

    Nascimento, Alessandro S.; Ferrarezi, Thiago; Catalano-Dupuy, Daniela L.; Ceccarelli, Eduardo A.; Polikarpov, Igor

    2006-01-01

    Crystals adequate for X-ray diffraction analysis have been prepared from L. interrogans ferredoxin-NADP + reductase. Ferredoxin-NADP + reductase (FNR) is an FAD-containing enzyme that catalyzes electron transfer between NADP(H) and ferredoxin. Here, results are reported of the recombinant expression, purification and crystallization of FNR from Leptospira interrogans, a parasitic bacterium of animals and humans. The L. interrogans FNR crystals belong to a primitive monoclinic space group and diffract to 2.4 Å resolution at a synchrotron source

  8. Crystallization and preliminary X-ray diffraction studies of ferredoxin reductase from Leptospira interrogans

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, Alessandro S.; Ferrarezi, Thiago [Instituto de Física de São Carlos, Universidade de São Paulo, Av. Trabalhador Saocarlense 400, São Carlos, SP, 13560-970 (Brazil); Catalano-Dupuy, Daniela L.; Ceccarelli, Eduardo A. [Facultad de Ciencias Bioquímicas y Farmacéuticas, Molecular Biology Division, Instituto de Biología Molecular y Celular de Rosario (IBR), CONICET, Universidad Nacional de Rosario, Suipacha 531, S2002LRK Rosario (Argentina); Polikarpov, Igor, E-mail: ipolikarpov@if.sc.usp.br [Instituto de Física de São Carlos, Universidade de São Paulo, Av. Trabalhador Saocarlense 400, São Carlos, SP, 13560-970 (Brazil)

    2006-07-01

    Crystals adequate for X-ray diffraction analysis have been prepared from L. interrogans ferredoxin-NADP{sup +} reductase. Ferredoxin-NADP{sup +} reductase (FNR) is an FAD-containing enzyme that catalyzes electron transfer between NADP(H) and ferredoxin. Here, results are reported of the recombinant expression, purification and crystallization of FNR from Leptospira interrogans, a parasitic bacterium of animals and humans. The L. interrogans FNR crystals belong to a primitive monoclinic space group and diffract to 2.4 Å resolution at a synchrotron source.

  9. Crystallization and preliminary X-ray diffraction analysis of mevalonate kinase from Methanosarcina mazei

    International Nuclear Information System (INIS)

    Zhuang, Ningning; Seo, Kyung Hye; Chen, Cong; Zhou, Jia; Kim, Seon Won; Lee, Kon Ho

    2012-01-01

    Recombinant mevalonate kinase from M. mazei has been crystallized. Diffraction data were collected to 2.08 Å resolution. Mevalonate kinase (MVK), which plays an important role in catalysing the biosynthesis of isoprenoid compounds derived from the mevalonate pathway, transforms mevalonate to 5-phosphomevalonate using ATP as a cofactor. Mevalonate kinase from Methanosarcina mazei (MmMVK) was expressed in Escherichia coli, purified and crystallized for structural analysis. Diffraction-quality crystals of MmMVK were obtained by the vapour-diffusion method using 0.32 M MgCl 2 , 0.08 M bis-tris pH 5.5, 16%(w/v) PEG 3350. The crystals belonged to space group P2 1 2 1 2, with unit-cell parameters a = 97.11, b = 135.92, c = 46.03 Å. Diffraction data were collected to 2.08 Å resolution

  10. Crystallization and preliminary X-ray diffraction analysis of the middle domain of Paip1

    International Nuclear Information System (INIS)

    Kanaan, Ahmad Seif; Frank, Filipp; Maedler-Kron, Chelsea; Verma, Karan; Sonenberg, Nahum; Nagar, Bhushan

    2009-01-01

    The crystallization of the putative MIF4G domain of Paip1 is described. The crystals belonged to the monoclinic space group P2 1 and diffracted X-rays to beyond 2.2 Å resolution. The poly(A)-binding protein (PABP) simultaneously interacts with the poly(A) tail of mRNAs and the scaffolding protein eIF4G to mediate mRNA circularization, resulting in stimulation of protein translation. PABP is regulated by the PABP-interacting protein Paip1. Paip1 is thought to act as a translational activator in 5′ cap-dependent translation by interacting with PABP and the initiation factors eIF4A and eIF3. Here, the crystallization and preliminary diffraction analysis of the middle domain of Paip1 (Paip1M), which produces crystals that diffract to a resolution of 2.2 Å, are presented

  11. Lattice effects in YVO3 single crystal

    NARCIS (Netherlands)

    Marquina, C; Sikora, M; Ibarra, MR; Nugroho, AA; Palstra, TTM

    In this paper we report on the lattice effects in the Mott insulator yttrium orthovanadate (YVO3). Linear thermal expansion and magnetostriction experiments have been performed on a single crystal, in the temperature range from 5 K to room temperature. The YVO3 orders antiferromagnetically at T-N =

  12. Method for manufacturing a single crystal nanowire

    NARCIS (Netherlands)

    van den Berg, Albert; Bomer, Johan G.; Carlen, Edwin; Chen, S.; Kraaijenhagen, Roderik Adriaan; Pinedo, Herbert Michael

    2013-01-01

    A method for manufacturing a single crystal nano-structure is provided comprising the steps of providing a device layer with a 100 structure on a substrate; providing a stress layer onto the device layer; patterning the stress layer along the 110 direction of the device layer; selectively removing

  13. Method for manufacturing a single crystal nanowire

    NARCIS (Netherlands)

    van den Berg, Albert; Bomer, Johan G.; Carlen, Edwin; Chen, S.; Kraaijenhagen, R.A.; Pinedo, Herbert Michael

    2010-01-01

    A method for manufacturing a single crystal nano-structure is provided comprising the steps of providing a device layer with a 100 structure on a substrate; providing a stress layer onto the device layer; patterning the stress layer along the 110 direction of the device layer; selectively removing

  14. X-ray Excited Optical Fluorescence and Diffraction Imaging of Reactivity and Crystallinity in a Zeolite Crystal : Crystallography and Molecular Spectroscopy in One

    NARCIS (Netherlands)

    Ristanovic, Zoran; Hofmann, Jan P; Richard, Marie-Ingrid; Jiang, Tao; Chahine, Gilbert A; Schülli, Tobias U; Meirer, Florian; Weckhuysen, Bert M

    2016-01-01

    Structure-activity relationships in heterogeneous catalysis are challenging to be measured on a single-particle level. For the first time, one X-ray beam is used to determine the crystallographic structure and reactivity of a single zeolite crystal. The method generates μm-resolved X-ray diffraction

  15. X-ray diffraction observations of a charge-density-wave order in superconducting ortho-II YBa2Cu3O6.54 single crystals in zero magnetic field

    DEFF Research Database (Denmark)

    Blackburn, E.; Chang, J.; Hücker, M.

    2013-01-01

    X-ray diffraction measurements show that the high-temperature superconductor YBa2Cu3O6.54, with ortho-II oxygen order, has charge-density-wave order in the absence of an applied magnetic field. The dominant wave vector of the charge density wave is qCDW=(0,0.328(2),0.5), with the in-plane component...

  16. Measuring the diffraction properties of an imaging quartz(211) crystal

    Energy Technology Data Exchange (ETDEWEB)

    Haugh, M. J.; Jacoby, K. D.; Koch, J. A. [National Security Technologies, LLC, Livermore, California 94550 (United States); Chen, H.; Schneider, M. B. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, California 94550 (United States); Hill, K. W. [Princeton Plasma Physics Laboratory, Princeton, New Jersey 08543 (United States)

    2016-06-15

    A dual goniometer X-ray system was used to measure the reflectivity curve for a spherically bent quartz(211) crystal. An analysis of the dual goniometer instrument response function for the rocking curve width measurement was developed and tested against the actual measurements. The rocking curve was measured at 4510.8 eV using the Ti Kα1 characteristic spectral line. The crystal is the dispersion element for a high resolution spectrometer used for plasma studies. It was expected to have a very narrow rocking curve width. The analysis showed that we could measure the upper bound for the rocking curve width of the Qz(211) crystal. The upper bound was 58 μrad giving a lower bound for the instrument resolving power E/ΔE = 34 000. Greatly improved insight into the dual goniometer operation and its limitations was achieved.

  17. Crystallization and preliminary X-ray diffraction analysis of central structure domains from mumps virus F protein

    International Nuclear Information System (INIS)

    Liu, Yueyong; Xu, Yanhui; Zhu, Jieqing; Qiu, Bingsheng; Rao, Zihe; Gao, George F.; Tien, Po

    2005-01-01

    Single crystals of the central structure domains from mumps virus F protein have been obtained by the hanging-drop vapour-diffusion method. A diffraction data set has been collected to 2.2 Å resolution. Fusion of members of the Paramyxoviridae family involves two glycoproteins: the attachment protein and the fusion protein. Changes in the fusion-protein conformation were caused by binding of the attachment protein to the cellular receptor. In the membrane-fusion process, two highly conserved heptad-repeat (HR) regions, HR1 and HR2, are believed to form a stable six-helix coiled-coil bundle. However, no crystal structure has yet been determined for this state in the mumps virus (MuV, a member of the Paramyxoviridae family). In this study, a single-chain protein consisting of two HR regions connected by a flexible amino-acid linker (named 2-Helix) was expressed, purified and crystallized by the hanging-drop vapour-diffusion method. A complete X-ray data set was obtained in-house to 2.2 Å resolution from a single crystal. The crystal belongs to space group C2, with unit-cell parameters a = 161.2, b = 60.8, c = 40.1 Å, β = 98.4°. The crystal structure will help in understanding the molecular mechanism of Paramyxoviridae family membrane fusion

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

    International Nuclear Information System (INIS)

    Emamzadah, Soheila; Petty, Tom J.; De Almeida, Victor; Nishimura, Taisuke; Joly, Jacques; Ferrer, Jean-Luc; Halazonetis, Thanos D.

    2009-01-01

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

  19. Thermal, mechanical, optical and dielectric properties of piperazinium hydrogen phosphite monohydrate NLO single crystal

    Science.gov (United States)

    Rajkumar, R.; Praveen Kumar, P.

    2018-05-01

    Optical transparent crystal of piperazinium hydrogen phosphite monohydrate (PHPM) was grown by slow evaporation method. The grown crystal was characterized by single crystal X-ray diffraction analysis and the crystal belongs to monoclinic system. The functional groups present in PHPM crystal were confirmed by FTIR analysis. UV-Visible spectrum shows that the PHPM crystal is transparent in the visible region. The mechanical behavior of PHPM crystal was characterized by Vickers hardness test. Thermal stability of PHPM crystal was analyzed by thermogravimetric analysis. Dielectric studies were also carried out for the grown crystal. The third-order nonlinear parameters such as nonlinear refractive index and nonlinear absorption coefficient have been calculated using Z scan technique.

  20. Synchrotron Bragg diffraction imaging characterization of synthetic diamond crystals for optical and electronic power device applications1 1

    Science.gov (United States)

    Tran Thi, Thu Nhi; Morse, J.; Caliste, D.; Fernandez, B.; Eon, D.; Härtwig, J.; Mer-Calfati, C.; Tranchant, N.; Arnault, J. C.; Lafford, T. A.; Baruchel, J.

    2017-01-01

    Bragg diffraction imaging enables the quality of synthetic single-crystal diamond substrates and their overgrown, mostly doped, diamond layers to be characterized. This is very important for improving diamond-based devices produced for X-ray optics and power electronics applications. The usual first step for this characterization is white-beam X-ray diffraction topography, which is a simple and fast method to identify the extended defects (dislocations, growth sectors, boundaries, stacking faults, overall curvature etc.) within the crystal. This allows easy and quick comparison of the crystal quality of diamond plates available from various commercial suppliers. When needed, rocking curve imaging (RCI) is also employed, which is the quantitative counterpart of monochromatic Bragg diffraction imaging. RCI enables the local determination of both the effective misorientation, which results from lattice parameter variation and the local lattice tilt, and the local Bragg position. Maps derived from these parameters are used to measure the magnitude of the distortions associated with polishing damage and the depth of this damage within the volume of the crystal. For overgrown layers, these maps also reveal the distortion induced by the incorporation of impurities such as boron, or the lattice parameter variations associated with the presence of growth-incorporated nitrogen. These techniques are described, and their capabilities for studying the quality of diamond substrates and overgrown layers, and the surface damage caused by mechanical polishing, are illustrated by examples. PMID:28381981

  1. X-ray diffraction from single GaAs nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Biermanns, Andreas

    2012-11-12

    In recent years, developments in X-ray focussing optics have allowed to produce highly intense, coherent X-ray beams with spot sizes in the range of 100 nm and below. Together with the development of new experimental stations, X-ray diffraction techniques can now be applied to study single nanometer-sized objects. In the present work, X-ray diffraction is applied to study different aspects of the epitaxial growth of GaAs nanowires. Besides conventional diffraction methods, which employ X-ray beams with dimensions of several tens of {mu}m, special emphasis lies on the use of nanodiffraction methods which allow to study single nanowires in their as-grown state without further preparation. In particular, coherent X-ray diffraction is applied to measure simultaneously the 3-dimensional shape and lattice parameters of GaAs nanowires grown by metal-organic vapor phase epitaxy. It is observed that due to a high density of zinc-blende rotational twins within the nanowires, their lattice parameter deviates systematically from the bulk zinc-blende phase. In a second step, the initial stage in the growth of GaAs nanowires on Si (1 1 1) surfaces is studied. This nanowires, obtained by Ga-assisted growth in molecular beam epitaxy, grow predominantly in the cubic zinc-blende structure, but contain inclusions of the hexagonal wurtzite phase close to their bottom interface. Using nanodiffraction methods, the position of the different structural units along the growth axis is determined. Because the GaAs lattice is 4% larger than silicon, these nanowires release their lattice mismatch by the inclusion of dislocations at the interface. Whereas NWs with diameters below 50 nm are free of strain, a rough interface structure in nanowires with diameters above 100 nm prevents a complete plastic relaxation, leading to a residual strain at the interface that decays elastically along the growth direction. Finally, measurements on GaAs-core/InAs-shell nanowire heterostructures are presented

  2. Residual Stress Measurement of Coarse Crystal Grain in Aluminium Casting Alloy by Neutron Diffraction

    International Nuclear Information System (INIS)

    Nishida, Masayuki; Watanabe, Yoshitaka; Hanabusa, Takao

    2009-01-01

    Full text: Neutron stress measurement can detect strain and stress information in deep region because of large penetration ability of neutron beams. The present paper describes procedure and results in the residual stress measurement of aluminium casting alloy by neutron diffraction. Usually, the aluminium casting alloy includes the large crystal grains. The existence of large crystal grains makes it difficult to estimate the residual stresses in highly accuracy. In this study, the modified three axial method using Hook's equation was employed for neutron stress measurement. These stress measurements were performed under the two kinds of new techniques. One is a rocking curve method to calculate the principal strains in three directions. The peak profiles which appear discretely on rocking curves were translated to principle stresses by the Bragg law and the basic elastic theory. Another is the consideration of measurement positions and the edge effect in the neutron irradiated area (volume gage). The edge effect generates the errors of 2θ-peak position in the neutron stress measurement. In this study, the edge effect was investigated in detail by a small bit of copper single crystal. The copper bit was moved and scanned on three dimensionally within the gage volume. Furthermore, the average strains of symmetrical positions are measure by the sample turning at 180 degrees, because the error distributions of the 2θ-peak position followed to positions inside the gage volume. Form these results of this study, the residual stresses in aluminium casting alloy which includes the large crystal grains were possible to estimate by neutron stress measurement with the rocking curve method and the correction of the edge effect. (author)

  3. Crystallization and diffraction analysis of thioredoxin reductase from Streptomyces coelicolor

    Czech Academy of Sciences Publication Activity Database

    Koháryová, M.; Brynda, Jiří; Řezáčová, Pavlína; Kollárová, M.

    F67, č. 8 (2011), s. 917-921 ISSN 1744-3091 Institutional research plan: CEZ:AV0Z40550506; CEZ:AV0Z50520514 Keywords : flavoenzymes * potential antibiotic target * crystallization Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 0.506, year: 2011

  4. Micromanipulation and pick-up system for X-Ray diffraction characterization of micrometer-sized single particles

    International Nuclear Information System (INIS)

    Takeichi, Y; Inami, N; Saito, K; Otori, H; Sagayama, R; Kumai, R; Ono, K; Ueno, T

    2014-01-01

    We describe a micromanipulation and pick-up system for preparing a micrometer-sized single particle for X-ray diffraction characterization. Combining a microgripper based on microelectromechanical systems, piezo-motor-driven linear stages, and a gamepad, the system provides precise and intuitive handling of the object. Single-crystal X-ray diffraction measurements of Sm-Fe-N permanent magnet were performed using this system. We also describe a method to distinguish crystallographically homogeneous particles found in powder-form samples.

  5. Multiple x-ray diffraction applied to the study of crystal impurities

    International Nuclear Information System (INIS)

    Cardoso, L.P.

    1983-06-01

    The x-ray multiple diffraction technique is used in the study of impurities concentration and localization in the crystal lattice, implemented with the fundamental observation that the impurities cannot be distributed with the same spatial group symmetry of the crystal. This fact could introduce scattered intensity in the crystal reciprocal lattice forbidden nodes. This effect was effectively observed in multiple diffraction diagrams, where a reinforcement of the scattered intensity in the pure crystal is produced, when choosing conveniently the involved reflections. The reflectivity theory was developed in the kinematic case, which take into account the scattering by the impurities atoms, and the analysis showed that, in the first approximation, the impurities can influence both in the allowed and forbidden positions for the pure crystal. (L.C.J.A.)

  6. Crystallization and diffraction analysis of β-N-acetylhexosaminidase from Aspergillus oryzae

    International Nuclear Information System (INIS)

    Vaněk, Ondřej; Brynda, Jiří; Hofbauerová, Kateřina; Kukačka, Zdeněk; Pachl, Petr; Bezouška, Karel; Řezáčová, Pavlína

    2011-01-01

    The fungal β-N-acetylhexosaminidase from A. oryzae was crystallized and diffraction data were collected from two crystal forms to 3.2 and 2.4 Å resolution, respectively. Fungal β-N-acetylhexosaminidases are enzymes that are used in the chemoenzymatic synthesis of biologically interesting oligosaccharides. The enzyme from Aspergillus oryzae was produced and purified from its natural source and crystallized using the hanging-drop vapour-diffusion method. Diffraction data from two crystal forms (primitive monoclinic and primitive tetragonal) were collected to resolutions of 3.2 and 2.4 Å, respectively. Electrophoretic and quantitative N-terminal protein-sequencing analyses confirmed that the crystals are formed by a complete biologically active enzyme consisting of a glycosylated catalytic unit and a noncovalently attached propeptide

  7. Purification, crystallization and preliminary X-ray diffraction studies of parakeet (Psittacula krameri) haemoglobin

    International Nuclear Information System (INIS)

    Jaimohan, S. M.; Naresh, M. D.; Arumugam, V.; Mandal, A. B.

    2009-01-01

    Parakeet (Psittacula krameri) haemoglobin has been purified and crystallized under low salt buffered conditions. Preliminary analysis of the crystal that belonged to monoclinic system (C2) is reported. Birds often show efficient oxygen management in order to meet the special demands of their metabolism. However, the structural studies of avian haemoglobins (Hbs) are inadequate for complete understanding of the mechanism involved. Towards this end, purification, crystallization and preliminary X-ray diffraction studies have been carried out for parakeet Hb. Parakeet Hb was crystallized as the met form in low-salt buffered conditions after extracting haemoglobin from crude blood by microcentrifugation and purifying the sample by column chromatography. Good-quality crystals were grown from 10% PEG 3350 and a crystal diffracted to about 2.8 Å resolution. Preliminary diffraction data showed that the Hb crystal belonged to the monoclinic system (space group C2), with unit-cell parameters a = 110.68, b = 64.27, c = 56.40 Å, β = 109.35°. Matthews volume analysis indicated that the crystals contained a half-tetramer in the asymmetric unit

  8. Radiation effects in corundum single crystals

    International Nuclear Information System (INIS)

    Gevorkyan, V.A.; Harutunyan, V.V.; Hakhverdyan, E.A.

    2005-01-01

    On the basis of new experimental results and analysis of publications it is shown that in the lattice of corundum crystals the high-energy particles create stable structural defects due to knocking out of atoms from normal sites of the anionic sublattice; this leads to the formation of F and F '+ centers as well as to other complex [Al i '+ F] type color centers. The essence of 'radiation memory' effect in corundum single crystals is that the high-energy particles irradiation, annealing at high temperatures and additional irradiation by X-rays result in the restoration of some spectral bands of the optical absorption in the range 200-650 nm

  9. Single Crystal Filters for Neutron Spectrometry

    International Nuclear Information System (INIS)

    Habib, N.

    2008-01-01

    A study of neutron transmission properties trough a large single crystals specimens of Si, Ge, Pb, Bi and sapphire at 300 K and 80 K have been made for a wide range of neutron energies. The effectiveness of such filters is given by the ratio of the total cross-section of unwanted epithermal neutrons to that the desired thermal neutron beam and by the optimum choice of the crystal orientation, its mosaic spread, thickness and temperature.Our study indicates that sapphire is significantly more effective than the others for a wide range of neutron energies

  10. Femtosecond X-ray diffraction from two-dimensional protein crystals

    Directory of Open Access Journals (Sweden)

    Matthias Frank

    2014-03-01

    Full Text Available X-ray diffraction patterns from two-dimensional (2-D protein crystals obtained using femtosecond X-ray pulses from an X-ray free-electron laser (XFEL are presented. To date, it has not been possible to acquire transmission X-ray diffraction patterns from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permit a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy approach at the Linac Coherent Light Source, Bragg diffraction was acquired to better than 8.5 Å resolution for two different 2-D protein crystal samples each less than 10 nm thick and maintained at room temperature. These proof-of-principle results show promise for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.

  11. New structural studies of liquid crystal by reflectivity and resonant X-ray diffraction

    International Nuclear Information System (INIS)

    Fernandes, P.

    2007-04-01

    This memory presents three structural studies of smectic Liquid Crystals by reflectivity and resonant diffraction of X-rays. It is divided in five chapters. In the first a short introduction to Liquid Crystals is given. In particular, the smectic phases that are the object of this study are presented. The second chapter is consecrated to the X-ray experimental techniques that were used in this work. The three last chapters present the works on which this thesis can be divided. Chapter three demonstrates on free-standing films of MHPOBC (historic liquid crystal that possesses the antiferroelectric sub-phases) the possibility to extend the technique of resonant X-ray diffraction to liquid crystals without resonant element. In the fourth chapter the structure of the B 2 liquid crystal phase of bent-core molecules (or banana molecules) is elucidated by using resonant X-ray diffraction combined with polarization analysis of the diffracted beam. A model of the polarization of the resonant beam diffracted by four different structures proposed for the B 2 phase is developed in this chapter. In the fifth chapter a smectic binary mixture presenting a very original critical point of phase separation is studied by X-ray reflectivity and optical microscopy. A concentration gradient in the direction perpendicular to the plane of the film seems to be induced by the free-standing film geometry. The results of a simplified model of the system are compatible with this interpretation

  12. Improved X-ray diffraction from Bacillus megaterium penicillin G acylase crystals through long cryosoaking dehydration

    International Nuclear Information System (INIS)

    Rojviriya, Catleya; Pratumrat, Thunyaluck; Saper, Mark A.; Yuvaniyama, Jirundon

    2011-01-01

    Penicillin G acylase from the Gram-positive bacterium B. megaterium was crystallized and X-ray diffraction from these crystals could be substantially improved by slight dehydration through a long cryo-soak. Penicillin G acylase from Bacillus megaterium (BmPGA) is currently used in the pharmaceutical industry as an alternative to PGA from Escherichia coli (EcPGA) for the hydrolysis of penicillin G to produce 6-aminopenicillanic acid (6-APA), a penam nucleus for semisynthetic penicillins. Despite the significant differences in amino-acid sequence between PGAs from Gram-positive and Gram-negative bacteria, a representative PGA structure of Gram-positive origin has never been reported. In this study, crystallization and diffraction studies of BmPGA are described. Poor diffraction patterns with blurred spots at higher resolution were typical for BmPGA crystals cryocooled after a brief immersion in cryoprotectant solution. Overnight soaking in the same cryo-solution substantially improved both the mosaicity and resolution limit through the establishment of a new crystal-packing equilibrium. A crystal of BmPGA diffracted X-rays to 2.20 Å resolution and belonged to the monoclinic space group P2 1 with one molecule of BmPGA in the asymmetric unit

  13. Preparation and characterization of single-crystal multiferroic nanofiber composites

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Zhaohui; Xiao, Zhen; Yin, Simin; Mai, Jiangquan; Liu, Zhenya; Xu, Gang; Li, Xiang; Shen, Ge [State Key Lab of Silicon Materials, Department of Material Science and Engineering, Cyrus Tang Center for Sensor Materials and Applications, Zhejiang University, Hangzhou 310027 (China); Han, Gaorong, E-mail: hgr@zju.edu.cn [State Key Lab of Silicon Materials, Department of Material Science and Engineering, Cyrus Tang Center for Sensor Materials and Applications, Zhejiang University, Hangzhou 310027 (China)

    2013-03-05

    Graphical abstract: One-dimensional single-crystal multiferroic composites composed of PbTiO{sub 3} nanofiber-CoFe{sub 2}O{sub 4} nanodot have been prepared for the first time by a facile in situ solid state sintering method. The composites demonstrate ferroelectricity and ferromagnetism as well as strong coupling between them. Highlights: ► 1D single-crystal multiferroic PTO-CFO was prepared via in situ solid state sintering method. ► A simple epitaxial growth relation has been found between the PTO–CFO composites. ► The composites reveal ferroelectricity and ferromagnetism as well as coupling between them. -- Abstract: One-dimensional single-crystal multiferroic composites consisting of PbTiO{sub 3} (PTO) nanofiber-CoFe{sub 2}O{sub 4} (CFO) nanodot were prepared using an in situ solid state sintering method, where pre-perovskite PTO nanofibers and CFO nanodots were used as precursors. Structural analyses by using transmission electron microscopy, scanning electron microscopy and X-ray diffraction determined a epitaxial growth relation between the PTO nanofiber and the CFO nanodot. Ferromagnetism and ferroelectricity of the nanofiber composites were investigated by using vibarting sample magnetometer (VSM) and piezoresponse force microscopy (PFM)

  14. Crystallization and preliminary X-ray diffraction analysis of PAT, an acetyltransferase from Sulfolobus solfataricus

    International Nuclear Information System (INIS)

    Cho, Ching-Chang; Luo, Ching-Wei; Hsu, Chun-Hua

    2008-01-01

    PAT, an acetyltransferase from the archaeon S. solfataricus that specifically acetylates the chromatin protein Alba, was expressed, purified and crystallized. PAT is an acetyltransferase from the archaeon Sulfolobus solfataricus that specifically acetylates the chromatin protein Alba. The enzyme was expressed, purified and subsequently crystallized using the sitting-drop vapour-diffusion technique. Native diffraction data were collected to 1.70 Å resolution on the BL13C1 beamline of NSRRC from a flash-frozen crystal at 100 K. The crystals belonged to space group P2 1 2 1 2 1 , with unit-cell parameters a = 44.30, b = 46.59, c = 68.39 Å

  15. Neutron diffraction studies of a double-crystal ( plus n,-m) setting containing a fully asymmetric diffraction geometry (FAD) of a bent perfect crystal (BPC)

    Czech Academy of Sciences Publication Activity Database

    Mikula, Pavol; Vrána, Miroslav; Šaroun, Jan; Em, V.

    2017-01-01

    Roč. 32, Supl-1 (2017), s. 13-18 ISSN 0885-7156 R&D Projects: GA ČR GC16-08803J; GA MŠk LM2015048 Institutional support: RVO:61389005 Keywords : neutron diffraction * monochromator * bent perfect crystal Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 0.674, year: 2016

  16. Studies on various properties of pure and Li-doped Barium Hydrogen Phosphate (BHP) single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Nallamuthu, D. [Department of Physics, Aditanar College of Arts and Science, Tiruchendur 628216, Tamil Nadu (India); Selvarajan, P., E-mail: pselvarajanphy@yahoo.co.i [Department of Physics, Aditanar College of Arts and Science, Tiruchendur 628216, Tamil Nadu (India); Freeda, T.H. [Physics Research Centre, S.T. Hindu College, Nagercoil 629002 (India)

    2010-12-15

    Single crystals of pure and Li-doped barium hydrogen phosphate (BHP) were grown by solution method with gel technique. Various properties of the harvested crystals were studied by carrying out single crystal and powder XRD, FTIR, TG/DTA, microhardness and dielectric studies. Atomic absorption study was carried out for Li-doped BHP crystal to check the presence of Li dopants. Unit cell dimensions and diffracting planes of the grown crystals have been identified from XRD studies. Functional groups of the title compounds have been identified from FTIR studies. Density of the grown crystals was calculated using the XRD data. Thermal stability of the samples was checked by TG/DTA studies. Mechanical and dielectric characterizations of the harvested pure and Li-doped BHP crystals reveal the mechanical strength and ferroelectric transition. The observed results are reported and discussed.

  17. High resolution diffraction imaging of mercuric iodide: Demonstration of the necessity for alternate crystal processing techniques for highly purified material

    International Nuclear Information System (INIS)

    Steiner, B.; Berg, L. van den; Laor, U.

    1995-01-01

    The overall crystalline lattice uniformity in recently available, highly purified mercuric iodide single crystals has been shown to be impacted by crystal handling techniques that were previously satisfactory. High resolution diffraction imaging of the surface regularity of crystals of various levels of purity and growth orientation shows: (1) that the newer materials have a generally lower level of precipitates, (2) that the incidence of these precipitates is now closely correlated with growth direction, and (3) that the deformation resistance and resulting sensitivity to crystal handling procedures are also closely correlated with these factors in this soft material. As a result, gentler cutting and polishing procedures have been developed and are shown to be effective in preserving overall lattice regularity in the new material. The polishing required to remove residual surface scratches affect the lattice orientation of the softer, precipitate-free regions, while not affecting those regions with detectable levels of precipitates. These results correlate closely with the electrical properties of devices made from these crystals. Mercuric iodide single crystals have proved to be particularly useful for x and γ ray detectors because their room temperature operation allow for simple, efficient, and compact instrumentation

  18. Purification, crystallization and preliminary X-ray diffraction analysis of the RNA-dependent RNA polymerase from Thosea asigna virus

    International Nuclear Information System (INIS)

    Ferrero, Diego; Buxaderas, Mònica; Rodriguez, José F.; Verdaguer, Núria

    2012-01-01

    The RNA-dependent RNA polymerase of Thosea asigna virus has been purified and crystallized in two different crystal forms. Preliminary characterization of P2 1 2 1 2 and C222 1 crystals is reported. Co-crystallization experiments in the presence of lutetium produced a heavy-atom derivative suitable for structure determination. Thosea asigna virus (TaV) is a positive-sense, single-stranded RNA (ssRNA) virus that belongs to the Permutotetravirus genera within the recently created Permutotetraviridae family. The genome of TaV consists of an RNA segment of about 5.700 nucleotides with two open reading frames, encoding for the replicase and capsid protein. The particular TaV replicase does not contain N7-methyl transferase and helicase domains but includes a structurally unique RNA-dependent RNA polymerase (RdRp) with a sequence permutation in the domain where the active site is anchored. This architecture is also found in double-stranded RNA viruses of the Birnaviridae family. Here we report the purification and preliminary crystallographic studies TaV RdRp. The enzyme was crystallized by the sitting-drop vapour diffusion method using PEG 8K and lithium sulfate as precipitants. Two different crystal forms were obtained: native RdRp crystallized in space group P2 1 2 1 2 and diffracts up to 2.1 Å and the RdRp-Lu 3+ derivative co-crystals belong to the C222 1 space group, diffracting to 3.0 Å resolution. The structure of TaV RdRp represents the first structure of a non-canonical RdRp from ssRNA viruses

  19. Crystallization and preliminary X-ray diffraction analysis of rat autotaxin

    International Nuclear Information System (INIS)

    Day, Jacqueline E.; Hall, Troii; Pegg, Lyle E.; Benson, Timothy E.; Hausmann, Jens; Kamtekar, Satwik

    2010-01-01

    Autotaxin (ATX), a pyrophosphatase/phosphodiesterase enzyme, is a promising drug target for many indications and is only distantly related to enzymes of previously determined structure. Here, the cloning, expression, purification, crystallization and preliminary diffraction analysis of ATX are reported. Rat autotaxin has been cloned, expressed, purified to homogeneity and crystallized via hanging-drop vapour diffusion using PEG 3350 as precipitant and ammonium iodide and sodium thiocyanate as salts. The crystals diffracted to a maximum resolution of 2.05 Å and belonged to space group P1, with unit-cell parameters a = 53.8, b = 63.3, c = 70.5 Å, α = 98.8, β = 106.2, γ = 99.8°. Preliminary X-ray diffraction analysis indicated the presence of one molecule per asymmetric unit, with a solvent content of 47%

  20. Characterization of a polychromatic neutron beam diffracted by pyrolytic graphite crystals

    CERN Document Server

    Byun, S H; Choi, H D

    2002-01-01

    The beam spectrum for polychromatic neutrons diffracted by pyrolytic graphite crystals was characterized. The theoretical beam spectrum was obtained using the diffraction model for a mosaic crystal. The lattice vibration effects were included in the calculation using the reported vibration amplitude of the crystal and the measured time-of-flight spectra in the thermal region. The calculated beam spectrum was compared with the results obtained in the absence of thermal motion. The lattice vibration effects became more important for the higher diffraction orders and a large decrease in the neutron flux induced by the vibrations was identified in the epithermal region. The validity of the beam spectrum was estimated by comparing with the effective quantities determined from prompt gamma-ray measurements and Cd-ratios measured both for 1/nu and non-1/nu nuclides.

  1. Study of structural and optical properties of YAG and Nd:YAG single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Kostić, S. [Institute of Physics, University of Belgrade, P.O. Box 68, Pregrevica 118, Zemun, Belgrade (Serbia); Lazarević, Z.Ž., E-mail: lzorica@yahoo.com [Institute of Physics, University of Belgrade, P.O. Box 68, Pregrevica 118, Zemun, Belgrade (Serbia); Radojević, V. [Faculty of Technology and Metallurgy, University of Belgrade, Belgrade (Serbia); Milutinović, A.; Romčević, M.; Romčević, N.Ž. [Institute of Physics, University of Belgrade, P.O. Box 68, Pregrevica 118, Zemun, Belgrade (Serbia); Valčić, A. [Faculty of Technology and Metallurgy, University of Belgrade, Belgrade (Serbia)

    2015-03-15

    Highlights: • Transparent YAG and pale pink Nd:YAG single crystals were produced by the Czochralski technique. • Growth mechanisms and shape of the liquid/solid interface and incorporation of Nd{sup 3+} were studied. • The structure of the crystals was investigated by X-ray diffraction, Raman and IR spectroscopy. • The 15 Raman and 17 IR modes were observed. • The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. - Abstract: Yttrium aluminum garnet (YAG, Y{sub 3}Al{sub 5}O{sub 12}) and yttrium aluminum garnet doped with neodymium (Nd:YAG) single crystals were grown by the Czochralski technique. The critical diameter and the critical rate of rotation were calculated. Suitable polishing and etching solutions were determined. As a result of our experiments, the transparent YAG and pale pink Nd:YAG single crystals were produced. The obtained crystals were studied by X-ray diffraction, Raman and IR spectroscopy. The crystal structure was confirmed by XRD. The 15 Raman and 17 IR modes were observed. The Raman and IR spectroscopy results are in accordance with X-ray diffraction analysis. The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. The absence of a core was confirmed by viewing polished crystal slices. Also, it is important to emphasize that the obtained Nd:YAG single crystal has a concentration of 0.8 wt.% Nd{sup 3+} that is characteristic for laser materials.

  2. Irradiation creep in zirconium single crystals

    International Nuclear Information System (INIS)

    MacEwen, S.R.; Fidleris, V.

    1976-07-01

    Two identical single crystals of crystal bar zirconium have been creep tested in reactor. Both specimens were preirradiated at low stress to a dose of about 4 x 10 23 n/m 2 (E > 1 MeV), and were then loaded to 25 MPa. The first specimen was loaded with reactor at full power, the second during a shutdown. The loading strain for both crystals was more than an order of magnitude smaller than that observed when an identical unirradiated crystal was loaded to the same stress. Both crystals exhibited periods of primary creep, after which their creep rates reached nearly constant values when the reactor was at power. During shutdowns the creep rates decreased rapidly with time. Electron microscopy revealed that the irradiation damage consisted of prismatic dislocation loops, approximately 13.5 nm in diameter. Cleared channels, identified as lying on (1010) planes, were also observed. The results are discussed in terms of the current theories for flux enhanced creep in the light of the microstructures observed. (author)

  3. Disappearing Enantiomorphs: Single Handedness in Racemate Crystals.

    Science.gov (United States)

    Parschau, Manfred; Ernst, Karl-Heinz

    2015-11-23

    Although crystallization is the most important method for the separation of enantiomers of chiral molecules in the chemical industry, the chiral recognition involved in this process is poorly understood at the molecular level. We report on the initial steps in the formation of layered racemate crystals from a racemic mixture, as observed by STM at submolecular resolution. Grown on a copper single-crystal surface, the chiral hydrocarbon heptahelicene formed chiral racemic lattice structures within the first layer. In the second layer, enantiomerically pure domains were observed, underneath which the first layer contained exclusively the other enantiomer. Hence, the system changed from a 2D racemate into a 3D racemate with enantiomerically pure layers after exceeding monolayer-saturation coverage. A chiral bias in form of a small enantiomeric excess suppressed the crystallization of one double-layer enantiomorph so that the pure minor enantiomer crystallized only in the second layer. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. The discovery of X-ray diffraction by crystals and its great impact on science

    International Nuclear Information System (INIS)

    Mai Zhenhong

    2012-01-01

    In April 1912, Friedrich, Knipping and Laue discovered X-ray diffraction in a CuSO 4 crystal. Later, Laue derived the famous Laue equations which explain the diffraction phenomenon. For this, Laue was awarded a Nobel Prize for Physics in 1914. In 1912 W. H. Bragg and W. L. Bragg received news of Laue 's discovery, and from X-ray diffraction experiments in a ZnS crystal they derived the famous Bragg equation. For this work, father and son were together awarded the Nobel Prize for Physics in 1915, To commemorate the 100th anniversary of the discovery of X-ray diffraction, this article reviews the important contributions of the early pioneers and their historic impact on science and technology worldwide. (author)

  5. The density and compositional analysis of titanium doped sapphire single crystal grown by the Czocharlski method

    Science.gov (United States)

    Kusuma, H. H.; Ibrahim, Z.; Othaman, Z.

    2018-03-01

    Titanium doped sapphire (Ti:Al2O3) crystal has attracted attention not only as beautiful gemstones, but also due to their applications as high power laser action. It is very important crystal for tunable solid state laser. Ti:Al2O3 crystals have been success grown using the Czocharlski method with automatic diameter control (ADC) system. The crystals were grown with different pull rates. The structure of the crystal was characterized with X-Ray Diffraction (XRD). The density of the crystal was measurement based on the Archimedes principle and the chemical composition of the crystal was confirmed by the Energy Dispersive X-ray (EDX) Spectroscopy. The XRD patterns of crystals are showed single main peak with a high intensity. Its shows that the samples are single crystal. The Ti:Al2O3 grown with different pull rate will affect the distribution of the concentration of dopant Ti3+ and densities on the sapphire crystals boules as well on the crystal growth process. The increment of the pull rate will increase the percentage distribution of Ti3+ and on the densities of the Ti:Al2O3 crystal boules. This may be attributed to the speed factor of the pull rate of the crystal that then caused changes in the heat flow in the furnace and then causes the homogeneities is changed of species distribution of atoms along crystal.

  6. Isotopically pure single crystal epitaxial diamond films and their preparation

    International Nuclear Information System (INIS)

    Banholzer, W.F.; Anthony, T.R.; Williams, D.M.

    1992-01-01

    The present invention is directed to the production of single crystal diamond consisting of isotopically pure carbon-12 or carbon-13. In the present invention, isotopically pure single crystal diamond is grown on a single crystal substrate directly from isotopically pure carbon-12 or carbon-13. One method for forming isotopically pure single crystal diamond comprises the steps of placing in a reaction chamber a single substrate heated to an elevated diamond forming temperature. Another method for forming isotopically pure single crystal diamond comprises diffusing isotopically pure carbon-12 or carbon-13 through a metallic catalyst under high pressure to a region containing a single crystal substrate to form an isotopically pure single crystal diamond layer on said single crystal substrate

  7. Single-Crystal Diamond Nanobeam Waveguide Optomechanics

    Science.gov (United States)

    Khanaliloo, Behzad; Jayakumar, Harishankar; Hryciw, Aaron C.; Lake, David P.; Kaviani, Hamidreza; Barclay, Paul E.

    2015-10-01

    Single-crystal diamond optomechanical devices have the potential to enable fundamental studies and technologies coupling mechanical vibrations to both light and electronic quantum systems. Here, we demonstrate a single-crystal diamond optomechanical system and show that it allows excitation of diamond mechanical resonances into self-oscillations with amplitude >200 nm . The resulting internal stress field is predicted to allow driving of electron spin transitions of diamond nitrogen-vacancy centers. The mechanical resonances have a quality factor >7 ×105 and can be tuned via nonlinear frequency renormalization, while the optomechanical interface has a 150 nm bandwidth and 9.5 fm /√{Hz } sensitivity. In combination, these features make this system a promising platform for interfacing light, nanomechanics, and electron spins.

  8. Single-Crystal Diamond Nanobeam Waveguide Optomechanics

    Directory of Open Access Journals (Sweden)

    Behzad Khanaliloo

    2015-12-01

    Full Text Available Single-crystal diamond optomechanical devices have the potential to enable fundamental studies and technologies coupling mechanical vibrations to both light and electronic quantum systems. Here, we demonstrate a single-crystal diamond optomechanical system and show that it allows excitation of diamond mechanical resonances into self-oscillations with amplitude >200  nm. The resulting internal stress field is predicted to allow driving of electron spin transitions of diamond nitrogen-vacancy centers. The mechanical resonances have a quality factor >7×10^{5} and can be tuned via nonlinear frequency renormalization, while the optomechanical interface has a 150 nm bandwidth and 9.5  fm/sqrt[Hz] sensitivity. In combination, these features make this system a promising platform for interfacing light, nanomechanics, and electron spins.

  9. Bulk crystal growth and their effective third order nonlinear optical properties of 2-(4-fluorobenzylidene) malononitrile (FBM) single crystal

    Science.gov (United States)

    Priyadharshini, A.; Kalainathan, S.

    2018-04-01

    2-(4-fluorobenzylidene) malononitrile (FBM), an organic third order nonlinear (TONLO) single crystal with the dimensions of 32 × 7 × 11 mm3, has been successfully grown in acetone solution by slow evaporation technique at 35 °C. The crystal system (triclinic), space group (P-1) and crystalline purity of the titular crystal were measured by single crystal and powder X-ray diffraction, respectively. The molecular weight and the multiple functional groups of the FBM material were confirmed through the mass and FT-IR spectral analysis. UV-Vis-NIR spectral study enroles that the FBM crystal exhibits excellent transparency (83%) in the entire visible and near infra-red region with a wide bandgap 2.90 eV. The low dielectric constant (εr) value of FBM crystal is appreciable for microelectronics industry applications. Thermal stability and melting point (130.09 °C) were ascertained by TGA-DSC analysis. The laser-induced surface damage threshold (LDT) value of FBM specimen is found to be 2.14 GW/cm2, it is fairly good compared to other reported NLO crystals. The third - order nonlinear optical character of the FBM crystal was confirmed through the typical single beam Z-scan technique. All these finding authorized that the organic crystal of FBM is favorably suitable for NLO applications.

  10. Crystal growth and optical properties of Sm:CaNb2O6 single crystal

    International Nuclear Information System (INIS)

    Di Juqing; Xu Xiaodong; Xia Changtai; Zeng Huidan; Cheng Yan; Li Dongzhen; Zhou Dahua; Wu Feng; Cheng Jimeng; Xu Jun

    2012-01-01

    Highlights: ► Sm:CaNb 2 O 6 single crystal was grown by the Czochralski method. ► Thermal expansion coefficients and J–O parameters were calculated. ► We found that this crystal had high quantum efficiency of 97%. - Abstract: Sm:CaNb 2 O 6 single crystal has been grown by the Czochralski method. Its high-temperature X-ray powder diffraction, optical absorption, emission spectroscopic as well as lifetime have been studied. Thermal expansion coefficients (α), J–O parameters (Ω i ), radiative lifetime (τ rad ), branching ratios (β) and stimulated emission cross-sections (σ e ) were calculated. The quantum efficiency (η) was calculated to be 97%. The intense peak emission cross section at 610, 658 nm were calculated to be 2.40 × 10 −21 , 2.42 × 10 −21 cm 2 . These results indicate that Sm:CaNb 2 O 6 crystal has potential use in visible laser and photonic devices area.

  11. Single crystal spectrometer FOX at KENS

    International Nuclear Information System (INIS)

    Takahashi, M.

    2001-01-01

    Single crystal spectrometer FOX installed at H1 thermal neutron line on KENS has been renewed recently for the measurement of very weak scattering. We have installed a multidetector system of 36 linearly placed 3 He detectors with collimators instead of former four-circle diffractometer and scintillator detectors. Though the system is quite simple, a large two-dimensional reciprocal space is observed effectively with high S/N rate on new FOX. (author)

  12. X-ray diffraction from ideal mosaic crystals in external fields of certain types. I. Atomic displacements and the corresponding diffraction patterns

    International Nuclear Information System (INIS)

    Treushnikov, E.N.

    2000-01-01

    The problem of the theoretical description of X-ray diffraction from ideal mosaic crystals under the effect of various external fields has been formulated. Electric, magnetic, electromagnetic, and acoustic perturbations are considered. The atomic displacements in crystals under the effect of external fields and the types of the corresponding diffraction patterns are analyzed for various types of perturbations. The crystal classes are determined in which atomic displacements can be recorded experimentally. Diffraction patterns formed under the effect of various external factors are considered on the basis of the derived dependence of the structure factor on the characteristics of an applied force field

  13. Anisotropic light diffraction in crystals with a large acoustic-energy walk-off

    Science.gov (United States)

    Balakshy, V. I.; Voloshin, A. S.; Molchanov, V. Ya.

    2014-11-01

    The influence of energy walk-off in an acoustic beam on the characteristic of anisotropic Bragg diffraction of light has been investigated by the example of paratellurite crystal. The angular and frequency characteristics of acousto-optic diffraction have been calculated in wide ranges of ultrasound frequencies and Bragg angles using the modified Raman-Nath equations. It is shown that the walk-off of an acoustic beam may change (either widen or narrow) significantly the frequency and angular ranges. The calculation results have been experimentally checked on an acousto-optic cell made of 10.5°-cut paratellurite crystal.

  14. Crystals of DhaA mutants from Rhodococcus rhodochrous NCIMB 13064 diffracted to ultrahigh resolution: crystallization and preliminary diffraction analysis.

    Science.gov (United States)

    Stsiapanava, Alena; Koudelakova, Tana; Lapkouski, Mikalai; Pavlova, Martina; Damborsky, Jiri; Smatanova, Ivana Kuta

    2008-02-01

    The enzyme DhaA from Rhodococcus rhodochrous NCIMB 13064 belongs to the haloalkane dehalogenases, which catalyze the hydrolysis of haloalkanes to the corresponding alcohols. The haloalkane dehalogenase DhaA and its variants can be used to detoxify the industrial pollutant 1,2,3-trichloropropane (TCP). Three mutants named DhaA04, DhaA14 and DhaA15 were constructed in order to study the importance of tunnels connecting the buried active site with the surrounding solvent to the enzymatic activity. All protein mutants were crystallized using the sitting-drop vapour-diffusion method. The crystals of DhaA04 belonged to the orthorhombic space group P2(1)2(1)2(1), while the crystals of the other two mutants DhaA14 and DhaA15 belonged to the triclinic space group P1. Native data sets were collected for the DhaA04, DhaA14 and DhaA15 mutants at beamline X11 of EMBL, DESY, Hamburg to the high resolutions of 1.30, 0.95 and 1.15 A, respectively.

  15. Crystallization and preliminary diffraction studies of CBM3b of cellobiohydrolase 9A from Clostridium thermocellum

    Energy Technology Data Exchange (ETDEWEB)

    Jindou, Sadanari [Department of Molecular Microbiology and Biotechnology, Tel Aviv University 69978 (Israel); Petkun, Svetlana [Department of Molecular Microbiology and Biotechnology, Tel Aviv University 69978 (Israel); The Daniella Rich Institute for Structural Biology, Tel Aviv University 69978 (Israel); Shimon, Linda [Department of Chemical Research Support, The Weizmann Institute of Science, Rehovot 76100 (Israel); Bayer, Edward A. [Department of Biological Chemistry, The Weizmann Institute of Science, Rehovot 76100 (Israel); Lamed, Raphael; Frolow, Felix, E-mail: mbfrolow@post.tau.ac.il [Department of Molecular Microbiology and Biotechnology, Tel Aviv University 69978 (Israel); The Daniella Rich Institute for Structural Biology, Tel Aviv University 69978 (Israel)

    2007-12-01

    The cloning, expression, purification and crystallization of the CBM3b module of cellobiohydrolase 9A from C. thermocellum is described. The crystals diffract to 2.68 Å. Family 3 carbohydrate-binding modules (CBM3s) are associated with the scaffoldin subunit of the multi-enzyme cellulosome complex and with the family 9 glycoside hydrolases, which are multimodular enzymes that act on plant cell-wall polysaccharides, notably cellulose. Here, the crystallization of CBM3b from cellobiohydrolase 9A is reported. The crystals are tetragonal and belong to space group P4{sub 1} or P4{sub 3}. X-ray diffraction data for CBM3b have been collected to 2.68 Å resolution on beamline ID14-4 at the ESRF.

  16. Crystallization and preliminary X-ray diffraction analysis of the fructofuranosidase from Xanthophyllomyces dendrorhous

    International Nuclear Information System (INIS)

    Polo, Aitana; Linde, Dolores; Estévez, Marta; Fernández-Lobato, María; Sanz-Aparicio, Julia

    2010-01-01

    The invertase from X. dendrorhous has been purified, deglycosylated and crystallized and diffraction data have been collected to 2.3 Å resolution. Xanthophyllomyces dendrorhous invertase is an extracellular enzyme that releases β-fructose from the nonreducing termini of various β-d-fructofuranoside substrates. Its ability to produce neokestose by transglycosylation makes this enzyme an interesting research target for applications in industrial biotechnology. The native enzyme, which is highly glycosylated, failed to crystallize. Therefore, it was submitted to EndoH deglycosylating treatment and crystals were grown by vapour-diffusion methods. The crystals belonged to space group P2 1 2 1 2, with unit-cell parameters a = 75.29, b = 204.93, c = 146.25 Å. Several diffraction data sets were collected using a synchrotron source. Self-rotation function and gel-filtration experiments suggested that the enzyme is a dimer with twofold symmetry

  17. Crystallization and preliminary X-ray diffraction analysis of red clover necrotic mosaic virus

    International Nuclear Information System (INIS)

    Martin, Stanton L.; Guenther, Richard H.; Sit, Tim L.; Swartz, Paul D.; Meilleur, Flora; Lommel, Steven A.; Rose, Robert B.

    2010-01-01

    Virions of red clover necrotic mosaic virus have been purified and crystallized. The space group was determined to be I23, with unit-cell parameter a = 377.8 Å. The crystals diffracted to 4 Å resolution. Red clover necrotic mosaic virus (RCNMV) is a species that belongs to the Tombusviridae family of plant viruses with a T = 3 icosahedral capsid. RCNMV virions were purified and were crystallized for X-ray analysis using the hanging-drop vapor-diffusion method. Self-rotation functions and systematic absences identified the space group as I23, with two virions in the unit cell. The crystals diffracted to better than 4 Å resolution but were very radiation-sensitive, causing rapid decay of the high-resolution reflections. The data were processed to 6 Å in the analysis presented here

  18. A new approach of quantum mechanics for neutron single-slit diffraction

    International Nuclear Information System (INIS)

    Wu Xiangyao; Yang Jinghai; Liu Xiaojing; Wang Li; Liu Bing; Fan Xihui; Guo Yiqing

    2007-01-01

    Phenomena of electron, neutron, atomic and molecular diffraction have been studied in many experiments, and these experiments are explained by many theoretical works. We study neutron single-slit diffraction with a quantum mechanical approach. It is found that the obvious diffraction patterns can be obtained when the single slit width a is in the range of 3λ-60λ. We also find a new quantum effect of the thickness of single-slit which can make a large impact on the diffraction pattern. The new quantum effect predicted in our work can be tested by the neutron single-slit diffraction experiment. (authors)

  19. Tunable diffraction and self-defocusing in liquid-filled photonic crystal fibers

    DEFF Research Database (Denmark)

    Rosberg, Christian Romer; Bennet, Francis H.; Neshev, Dragomir N.

    2007-01-01

    We suggest and demonstrate a novel platform for the study of tunable nonlinear light propagation in two-dimensional discrete systems, based on photonic crystal fibers filled with high index nonlinear liquids. Using the infiltrated cladding region of a photonic crystal fiber as a nonlinear waveguide...... array, we experimentally demonstrate highly tunable beam diffraction and thermal self-defocusing, and realize a compact all-optical power limiter based on a tunable nonlinear response....

  20. How to distinguish perfect quasi-crystals from twins and other structures using diffraction experiments?

    International Nuclear Information System (INIS)

    Wolny, J.

    1992-01-01

    Performing diffraction experiments for various lengths of coherent scattering and using the scaling of peak intensities on a number of atoms one can experimentally distinguish quasi-crystals from the other structures (e.g. twins or random). For perfect quasi-crystals peak intensities scale as N 2 , for other structures this scaling depends on concentration of atoms, behaving critical for Penrose concentration. 3 figs., 8 refs. (author)

  1. Development of n- and p-type Doped Perovskite Single Crystals Using Solid-State Single Crystal Growth (SSCG) Technique

    Science.gov (United States)

    2017-10-09

    for AGG should be minimal. For this purpose, the seeds for AGG may also be provided externally. This process is called the solid-state single...bonding process . Figure 31 shows (a) the growth of one large single crystal from one small single crystal seed as well as (b) the growth of one...one bi-crystal seed : One large bi-crystal can be grown from one small bi-crystal by SSCG process . Fig. 32. Diffusion bonding process for

  2. Room-temperature serial crystallography using a kinetically optimized microfluidic device for protein crystallization and on-chip X-ray diffraction

    Directory of Open Access Journals (Sweden)

    Michael Heymann

    2014-09-01

    Full Text Available An emulsion-based serial crystallographic technology has been developed, in which nanolitre-sized droplets of protein solution are encapsulated in oil and stabilized by surfactant. Once the first crystal in a drop is nucleated, the small volume generates a negative feedback mechanism that lowers the supersaturation. This mechanism is exploited to produce one crystal per drop. Diffraction data are measured, one crystal at a time, from a series of room-temperature crystals stored on an X-ray semi-transparent microfluidic chip, and a 93% complete data set is obtained by merging single diffraction frames taken from different unoriented crystals. As proof of concept, the structure of glucose isomerase was solved to 2.1 Å, demonstrating the feasibility of high-throughput serial X-ray crystallography using synchrotron radiation.

  3. Preparation, crystallization, and preliminary X-ray diffraction study of mutant carboxypeptidase T containing the primary specificity pocket of carboxypeptidase B

    International Nuclear Information System (INIS)

    Akparov, V. Kh.; Grishin, A. M.; Timofeev, V. I.; Kuranova, I. P.

    2010-01-01

    Recombinant G215S, A251G, T257A, D260G, T262D mutant carboxypeptidase T from Thermoactinomyces vulgaris containing mutations in the primary specificity pocket was prepared and crystallized. Single crystals with a size of up to 0.3 mm were grown and investigated by X-ray diffraction. Recombinant mutant carboxypeptidase T containing the primary specificity subsite compositionally identical to that of pancreatic carboxypeptidase B crystallizes in the same space group as the natural enzyme. The crystals belong to sp. gr. P6 3 22; the unit-cell parameters are a = b = 157.867 A, c = 104.304 A, α = β = 90 deg., γ = 120 deg. X-ray diffraction data suitable for determining the three-dimensional structure at atomic resolution were collected from one crystal.

  4. Spall response of single-crystal copper

    Science.gov (United States)

    Turley, W. D.; Fensin, S. J.; Hixson, R. S.; Jones, D. R.; La Lone, B. M.; Stevens, G. D.; Thomas, S. A.; Veeser, L. R.

    2018-02-01

    We performed a series of systematic spall experiments on single-crystal copper in an effort to determine and isolate the effects of crystal orientation, peak stress, and unloading strain rate on the tensile spall strength. Strain rates ranging from 0.62 to 2.2 × 106 s-1 and peak shock stresses in the 5-14 GPa range, with one additional experiment near 50 GPa, were explored as part of this work. Gun-driven impactors, called flyer plates, generated flat top shocks followed by spall. This work highlights the effect of crystal anisotropy on the spall strength by showing that the spall strength decreases in the following order: [100], [110], and [111]. Over the range of stresses and strain rates explored, the spall strength of [100] copper depends strongly on both the strain rate and shock stress. Except at the very highest shock stress, the results for the [100] orientation show linear relationships between the spall strength and both the applied compressive stress and the strain rate. In addition, hydrodynamic computer code simulations of the spall experiments were performed to calculate the relationship between the strain rate near the spall plane in the target and the rate of free surface velocity release during the pullback. As expected, strain rates at the spall plane are much higher than the strain rates estimated from the free surface velocity release rate. We have begun soft recovery experiments and molecular dynamics calculations to understand the unusual recompression observed in the spall signature for [100] crystals.

  5. Unidirectional growth and characterization of L-arginine monohydrochloride monohydrate single crystals

    International Nuclear Information System (INIS)

    Sangeetha, K.; Babu, R. Ramesh; Bhagavannarayana, G.; Ramamurthi, K.

    2011-01-01

    Highlights: → L-Arginine monohydrochloride monohydrate (LAHCl) single crystal was grown successfully by unidirectional solution growth method for the first time. → High crystalline perfection was observed for UDS grown crystal compared to CS grown crystal. → The optical transparency and mechanical stability are high for UDS grown LAHCl single crystal. → Optical birefringence measurement on this material. → The piezoelectric resonance frequencies observation - first time observation on this material. - Abstract: L-Arginine monohydrochloride monohydrate (LAHCl) single crystals were grown successfully by conventional and unidirectional solution growth methods. The crystalline perfection of grown crystals was analyzed by high-resolution X-ray diffraction. The linear optical transmittance, mechanical stability of conventional and unidirectional grown LAHCl single crystals were analyzed and compared along (0 0 1) plane. The refractive index and birefringence of LAHCl single crystals were also measured using He-Ne laser source. From the dielectric studies, piezoelectric resonance frequencies were observed in kHz frequency range for both conventional and unidirectional grown LAHCl single crystals along (0 0 1) plane.

  6. Types of defect ordering in undoped and lanthanum-doped Bi2201 single crystals

    International Nuclear Information System (INIS)

    Martovitsky, V. P.

    2006-01-01

    Undoped and lanthanum-doped Bi2201 single crystals having a perfect average structure have been comparatively studied by x-ray diffraction. The undoped Bi2201 single crystals exhibit very narrow satellite reflections; their half-width is five to six times smaller than that of Bi2212 single crystals grown by the same technique. This narrowness indicates three-dimensional defect ordering in the former crystals. The lanthanumdoped Bi2201 single crystals with x = 0.7 and T c = 8-10 K exhibit very broad satellite reflections consisting of two systems (modulations) misoriented with respect to each other. The modulation-vector components of these two modulations are found to be q 1 = 0.237b* + 0.277c* and q 2 = 0.238b* + 0.037c*. The single crystals having a perfect average structure and a homogeneous average distribution of doping lanthanum consist of 70-to 80-A-thick layers that alternate along the c axis and have two different types of modulated superlattice. The crystals having a less perfect average structure also consist of alternating layers, but they have different lanthanum concentrations. The low value of T c in the undoped Bi2201 single crystals (9.5 K) correlates with three-dimensional defect ordering in them, and an increase in T c to 33 K upon lanthanum doping can be related to a thin-layer structure of these crystals and to partial substitution of lanthanum for the bismuth positions

  7. Validation of molecular crystal structures from powder diffraction data with dispersion-corrected density functional theory (DFT-D)

    International Nuclear Information System (INIS)

    Streek, Jacco van de; Neumann, Marcus A.

    2014-01-01

    The accuracy of 215 experimental organic crystal structures from powder diffraction data is validated against a dispersion-corrected density functional theory method. In 2010 we energy-minimized 225 high-quality single-crystal (SX) structures with dispersion-corrected density functional theory (DFT-D) to establish a quantitative benchmark. For the current paper, 215 organic crystal structures determined from X-ray powder diffraction (XRPD) data and published in an IUCr journal were energy-minimized with DFT-D and compared to the SX benchmark. The on average slightly less accurate atomic coordinates of XRPD structures do lead to systematically higher root mean square Cartesian displacement (RMSCD) values upon energy minimization than for SX structures, but the RMSCD value is still a good indicator for the detection of structures that deserve a closer look. The upper RMSCD limit for a correct structure must be increased from 0.25 Å for SX structures to 0.35 Å for XRPD structures; the grey area must be extended from 0.30 to 0.40 Å. Based on the energy minimizations, three structures are re-refined to give more precise atomic coordinates. For six structures our calculations provide the missing positions for the H atoms, for five structures they provide corrected positions for some H atoms. Seven crystal structures showed a minor error for a non-H atom. For five structures the energy minimizations suggest a higher space-group symmetry. For the 225 SX structures, the only deviations observed upon energy minimization were three minor H-atom related issues. Preferred orientation is the most important cause of problems. A preferred-orientation correction is the only correction where the experimental data are modified to fit the model. We conclude that molecular crystal structures determined from powder diffraction data that are published in IUCr journals are of high quality, with less than 4% containing an error in a non-H atom

  8. Growth and characterisation of lead iodide single crystals

    International Nuclear Information System (INIS)

    Tonn, Justus

    2012-01-01

    The work in hand deals with the growth and characterisation of lead iodide (PbI 2 ) single crystals. PbI 2 is regarded as a promising candidate for low-noise X- and gamma ray detection at room temperature. Its benefits if compared to conventional materials like HgI 2 , CdTe, Si, or GaAs lie in a band gap energy of 2.32 eV, an excellent ability to absorb radiation, and a high electrical resistivity. For an application of PbI 2 as detector material the growth and characterisation of crystals with high chemical and structural quality is extremely challenging. In light of this, the effectiveness of zone purification of the PbI 2 used for crystal growth was confirmed by spectroscopic analysis. Furthermore, technological aspects during processing of purified PbI 2 were investigated. With the help of thermal analysis, a correlation was found between the degree of exposing the source material to oxygen from the air and the structural quality of the resulting crystals. A hydrogen treatment was applied to PbI 2 as an effective method for the removal of oxidic pollutions, which resulted in a significant reduction of structural defects like polytypic growth and stress-induced cracking. The growth of PbI 2 single crystals was, among others, carried out by the Bridgman-Stockbarger method. In this context, much effort was put on the investigation of influences resulting from the design and preparation of ampoules. For the first time, crystal growth of PbI 2 was also carried out by the Czochralski method. If compared to the Bridgman-Stockbarger method, the Czochralski technique allowed a significantly faster growth of nearly crack-free crystals with a reproducible predetermination of crystallographic orientation. By an optimised sample preparation of PbI 2 , surface orientations perpendicular to the usually cleaved (0001) plane were realised. It is now possible to determine the material properties along directions which were so far not accessible. Thus, for example, the ratio of

  9. Dynamic Diffraction Studies on the Crystallization, Phase Transformation, and Activation Energies in Anodized Titania Nanotubes

    OpenAIRE

    Hani Albetran; Victor Vega; Victor M. Prida; It-Meng Low

    2018-01-01

    The influence of calcination time on the phase transformation and crystallization kinetics of anodized titania nanotube arrays was studied using in-situ isothermal and non-isothermal synchrotron radiation diffraction from room temperature to 900 °C. Anatase first crystallized at 400 °C, while rutile crystallized at 550 °C. Isothermal heating of the anodized titania nanotubes by an increase in the calcination time at 400, 450, 500, 550, 600, and 650 °C resulted in a slight reduction in anatase...

  10. Colour centre-free perovskite single crystals

    International Nuclear Information System (INIS)

    Petit, Pierre-Olivier; Petit, Johan; Goldner, Philippe; Viana, Bruno

    2009-01-01

    Yb 3+ :YAlO 3 (YAP) and Yb 3+ :GdAlO 3 (GAP) are interesting 1 μm high-power laser media thanks to their very good thermo-mechanical properties. However, as-grown perovskite single crystals exhibit colour centres. Parasitic thermal load generated by these centres is deleterious for high-power laser action and can lead to crystal damages. Moreover these defects decrease Yb 3+ lifetime. They are related to trapped holes on the oxygen network. In the present work, several schemes to remove colour centres are presented. Attention is focused on cerium codoping, thermal annealing under reducing atmosphere and growth of non-stoechiometric compounds.

  11. Crystal structure determination from powder diffraction data of the coumarin vanillin chalcone

    Czech Academy of Sciences Publication Activity Database

    Ghouili, A.; Rohlíček, Jan; Ayed, T.B.; Hassen, R.B.

    2014-01-01

    Roč. 29, č. 4 (2014), s. 361-365 ISSN 0885-7156 Grant - others:AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : chalcone * absorption spectra * powder diffraction * crystal structure determination * coumarin derivatives Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.636, year: 2014

  12. On a semiclassical analysis of high energy electron diffraction by imperfect crystals: the stacking fault

    International Nuclear Information System (INIS)

    Smith, A.E.; Chadderton, L.T.; Johnson, E.

    1978-01-01

    Electron diffraction amplitudes at the lower surface of a displaced sandwich crystal are obtained for the high energy limit in the real space formulation. Using semiclassical methods analytical approximations to a resulting overlap integral - central to the problem - are derived. (Auth.)

  13. Characterization of calcium crystals in Abelia using x-ray diffraction and electron microscopes

    Science.gov (United States)

    Localization, chemical composition, and morphology of calcium crystals in leaves and stems of Abelia mosanensis and A. ×grandiflora were analyzed with a variable pressure scanning electron microscope (VP-SEM) equipped with an X-ray diffraction system, low temperature SEM (LT-SEM) and a transmission ...

  14. Crystallization Kinetics of Nanocrystalline Materials by Combined X-ray Diffraction and Differential Scanning Calorimetry Experiments

    Czech Academy of Sciences Publication Activity Database

    Gil-González, E.; Perejón, A.; Sánchez-Jiménez, P. E.; Medina-Carrasco, S.; Kupčík, Jaroslav; Šubrt, Jan; Criado, J. M.; Pérez-Maqueda, L. A.

    2018-01-01

    Roč. 18, č. 5 (2018), s. 3107-3116 ISSN 1528-7483 Institutional support: RVO:61388980 Keywords : nanocrysalline alloys * combined X ray diffraction * crystallization kinetics Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 4.055, year: 2016

  15. On dislocation inhomogeneity of electroerosion crater zone in molybdenum single crystals

    International Nuclear Information System (INIS)

    Larikov, L.N.; Dubovitskaya, N.V.; Zakharov, S.M.

    1979-01-01

    Methods of diffraction electron microscopy, X-ray analysis and microhardness measurements have been applied to study the inhomogeneity of dislocation structure of the electroerosion crater zone in molybdenum single crystals. Microhardness inhomogeneous distribution in this zone is established, conditioned by changes in dislocation structure as a result of the development of thermally activated processes of the plastic deformation and dynamic recovery. Dislocationless channels are detected in predeformed crystals

  16. Evanescent Properties of Optical Diffraction from 2-Dimensional Hexagonal Photonic Crystals and Their Sensor Applications.

    Science.gov (United States)

    Liao, Yu-Yang; Chen, Yung-Tsan; Chen, Chien-Chun; Huang, Jian-Jang

    2018-04-03

    The sensitivity of traditional diffraction grating sensors is limited by the spatial resolution of the measurement setup. Thus, a large space is required to improve sensor performance. Here, we demonstrate a compact hexagonal photonic crystal (PhC) optical sensor with high sensitivity. PhCs are able to diffract optical beams to various angles in azimuthal space. The critical wavelength that satisfies the phase matching or becomes evanescent was used to benchmark the refractive index of a target analyte applied on a PhC sensor. Using a glucose solution as an example, our sensor demonstrated very high sensitivity and a low limit of detection. This shows that the diffraction mechanism of hexagonal photonic crystals can be used for sensors when compact size is a concern.

  17. Growth of single crystals of BaFe12O19 by solid state crystal growth

    International Nuclear Information System (INIS)

    Fisher, John G.; Sun, Hengyang; Kook, Young-Geun; Kim, Joon-Seong; Le, Phan Gia

    2016-01-01

    Single crystals of BaFe 12 O 19 are grown for the first time by solid state crystal growth. Seed crystals of BaFe 12 O 19 are buried in BaFe 12 O 19 +1 wt% BaCO 3 powder, which are then pressed into pellets containing the seed crystals. During sintering, single crystals of BaFe 12 O 19 up to ∼130 μm thick in the c-axis direction grow on the seed crystals by consuming grains from the surrounding polycrystalline matrix. Scanning electron microscopy-energy dispersive spectroscopy analysis shows that the single crystal and the surrounding polycrystalline matrix have the same chemical composition. Micro-Raman scattering shows the single crystal to have the BaFe 12 O 19 structure. The optimum growth temperature is found to be 1200 °C. The single crystal growth behavior is explained using the mixed control theory of grain growth. - Highlights: • Single crystals of BaFe 12 O 19 are grown by solid state crystal growth. • A single crystal up to ∼130 μm thick (c-axis direction) grows on the seed crystal. • The single crystal and surrounding ceramic matrix have similar composition. • Micro-Raman scattering shows the single crystal has the BaFe 12 O 19 structure.

  18. Crystallization and diffraction analysis of the serpin IRS-2 from the hard tick Ixodes ricinus

    International Nuclear Information System (INIS)

    Kovářová, Zuzana; Chmelař, Jindřich; Šanda, Miloslav; Brynda, Jiří; Mareš, Michael; Řezáčová, Pavlína

    2010-01-01

    Cleavage of the serpin IRS-2 from the hard tick I. ricinus by contaminating proteolytic activity mimicked the specific processing of the serpin by its target protease and resulted in a more stable form of the serpin which produced crystals that diffracted to 1.8 Å resolution. IRS-2 from the hard tick Ixodes ricinus belongs to the serpin family of protease inhibitors. It is produced in the salivary glands of the tick and its anti-inflammatory activity suggests that it plays a role in parasite–host interaction. Recombinant IRS-2 prepared by heterologous expression in a bacterial system was crystallized using the hanging-drop vapour-diffusion method. The crystals belonged to the primitive tetragonal space group P4 3 and diffracted to 1.8 Å resolution. Mass-spectrometric and electrophoretic analyses revealed that IRS-2 was cleaved by contaminating proteases during crystallization. This processing of IRS-2 mimicked the specific cleavage of the serpin by its target protease and resulted in a more stable form (the so-called relaxed conformation), which produced well diffracting crystals. Activity profiling with specific substrates and inhibitors demonstrated traces of serine and cysteine proteases in the protein stock solution

  19. The purification, crystallization and preliminary X-ray diffraction analysis of dihydrodipicolinate synthase from Clostridium botulinum

    International Nuclear Information System (INIS)

    Dobson, Renwick C. J.; Atkinson, Sarah C.; Gorman, Michael A.; Newman, Janet M.; Parker, Michael W.; Perugini, Matthew A.

    2008-01-01

    Dihydrodipicolinate synthase (DHDPS), an enzyme in the lysine-biosynthetic pathway, is a promising target for antibiotic development against pathogenic bacteria. Here, the expression, purification, crystallization and preliminary diffraction analysis of DHDPS from C. botulinum are reported. In recent years, dihydrodipicolinate synthase (DHDPS; EC 4.2.1.52) has received considerable attention from both mechanistic and structural viewpoints. This enzyme, which is part of the diaminopimelate pathway leading to lysine, couples (S)-aspartate-β-semialdehyde with pyruvate via a Schiff base to a conserved active-site lysine. In this paper, the expression, purification, crystallization and preliminary X-ray diffraction analysis of DHDPS from Clostridium botulinum, an important bacterial pathogen, are presented. The enzyme was crystallized in a number of forms, predominantly using PEG precipitants, with the best crystal diffracting to beyond 1.9 Å resolution and displaying P4 2 2 1 2 symmetry. The unit-cell parameters were a = b = 92.9, c = 60.4 Å. The crystal volume per protein weight (V M ) was 2.07 Å 3 Da −1 , with an estimated solvent content of 41%. The structure of the enzyme will help guide the design of novel therapeutics against the C. botulinum pathogen

  20. Nonlinear magnetoelectric effect in paraelectric state of Co4Nb2O9 single crystal

    Czech Academy of Sciences Publication Activity Database

    Cao, Ym.; Deng, Gc.; Beran, Přemysl; Feng, Zj.; Kang, Bj.; Zhang, Jc.; Guiblin, N.; Dkhil, B.; Ren, W.; Cao, Sx.

    2017-01-01

    Roč. 7, č. 10 (2017), č. článku 14079. ISSN 2045-2322 Institutional support: RVO:61389005 Keywords : magnetoelectric * single crystal * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 4.259, year: 2016

  1. Dynamical electron diffraction simulation for non-orthogonal crystal system by a revised real space method.

    Science.gov (United States)

    Lv, C L; Liu, Q B; Cai, C Y; Huang, J; Zhou, G W; Wang, Y G

    2015-01-01

    In the transmission electron microscopy, a revised real space (RRS) method has been confirmed to be a more accurate dynamical electron diffraction simulation method for low-energy electron diffraction than the conventional multislice method (CMS). However, the RRS method can be only used to calculate the dynamical electron diffraction of orthogonal crystal system. In this work, the expression of the RRS method for non-orthogonal crystal system is derived. By taking Na2 Ti3 O7 and Si as examples, the correctness of the derived RRS formula for non-orthogonal crystal system is confirmed by testing the coincidence of numerical results of both sides of Schrödinger equation; moreover, the difference between the RRS method and the CMS for non-orthogonal crystal system is compared at the accelerating voltage range from 40 to 10 kV. Our results show that the CMS method is almost the same as the RRS method for the accelerating voltage above 40 kV. However, when the accelerating voltage is further lowered to 20 kV or below, the CMS method introduces significant errors, not only for the higher-order Laue zone diffractions, but also for zero-order Laue zone. These indicate that the RRS method for non-orthogonal crystal system is necessary to be used for more accurate dynamical simulation when the accelerating voltage is low. Furthermore, the reason for the increase of differences between those diffraction patterns calculated by the RRS method and the CMS method with the decrease of the accelerating voltage is discussed. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

  2. Purification, crystallization and preliminary diffraction studies of an ectromelia virus glutaredoxin

    International Nuclear Information System (INIS)

    Bacik, John-Paul; Brigley, Angela M.; Channon, Lisa D.; Audette, Gerald F.; Hazes, Bart

    2005-01-01

    Ectromelia virus glutaredoxin has been crystallized in the presence of the reducing agent DTT. A diffraction data set has been collected and processed to 1.8 Å resolution. Ectromelia, vaccinia, smallpox and other closely related viruses of the orthopoxvirus genus encode a glutaredoxin gene that is not present in poxviruses outside of this genus. The vaccinia glutaredoxin O2L has been implicated as the reducing agent for ribonucleotide reductase and may thus play an important role in viral deoxyribonucleotide synthesis. As part of an effort to understand nucleotide metabolism by poxviruses, EVM053, the O2L ortholog of the ectromelia virus, has been crystallized. EVM053 crystallizes in space group C222 1 , with unit-cell parameters a = 61.98, b = 67.57, c = 108.55 Å. Diffraction data have been processed to 1.8 Å resolution and a self-rotation function indicates that there are two molecules per asymmetric unit

  3. Crystallization and X-ray diffraction analysis of dihydropyrimidinase from Saccharomyces kluyveri

    International Nuclear Information System (INIS)

    Dobritzsch, Doreen; Andersen, Birgit; Piškur, Jure

    2005-01-01

    Dihydropyrimidinase from the yeast S. kluyveri was crystallized by vapour diffusion. The crystals belong to space group P2 1 (unit-cell parameters a = 91.0, b = 73.0, c = 161.4 Å, β = 91.4°) and diffracted to 2.6 Å resolution. Dihydropyrimidinase (EC 3.5.2.2) catalyzes the second step in the reductive pathway of pyrimidine degradation, the hydrolysis of 5,6-dihydrouracil and 5,6-dihydrothymine to the corresponding N-carbamylated β-amino acids. Crystals of the recombinant enzyme from the yeast Saccharomyces kluyveri diffracting to 2.6 Å at a synchrotron-radiation source have been obtained by the hanging-drop vapour-diffusion method. They belong to space group P2 1 (unit-cell parameters a = 91.0, b = 73.0, c = 161.4 Å, β = 91.4°), with one homotetramer per asymmetric unit

  4. Crystallization and preliminary X-ray diffraction analysis of alanine racemase from Pseudomonas putida YZ-26

    International Nuclear Information System (INIS)

    Liu, Junlin; Feng, Lei; Shi, Yawei; Feng, Wei

    2012-01-01

    A recombinant alanine racemase from the Pseudomonas putida YZ-26, has been crystallized by the sitting-drop vapor-diffusion method and X-ray diffraction data were collected to 2.4 Å. A recombinant form of alanine racemase (Alr) from Pseudomonas putida YZ-26 has been crystallized by the sitting-drop vapour diffusion method. X-ray diffraction data were collected to 2.4 Å resolution. The crystals belong to the space group C222 1 , with unit-cell parameters a = 118.08, b = 141.86, c = 113.83 Å, and contain an Alr dimer in the asymmetric unit. The Matthews coefficient and the solvent content were calculated to be 2.8 Å 3 Da −1 and approximately 50%, respectively

  5. On the neutron diffraction in a crystal in the field of a standing laser wave

    International Nuclear Information System (INIS)

    Grigoryan, K.K.; Hayrapetyan, A.G.; Petrosyan, R.G.

    2010-01-01

    The possibility of high-energy neutron diffraction in a crystal is shown by applying the solution of time-dependent Schroedinger equation for a neutron in the field of a standing laser wave. The scattering picture is examined within the framework of non-stationary S-matrix theory, where the neutron-laser field interaction is considered exactly and the neutron-crystal interaction is considered as a perturbation described by Fermi pseudopotential (Farri representation). The neutron-crystal interaction is elastic, and the neutron-laser field interaction has both inelastic and elastic behaviors which results in the observation of an analogous to the Kapitza-Dirac effect for neutrons. The neutron scattering probability is calculated and the analysis of the results are adduced. Both inelastic and elastic diffraction conditions are obtained and the formation of a 'sublattice' is illustrated in the process of neutron-photon-phonon elastic interaction.

  6. A program for the derivation of crystal unit cell parameters from X-ray powder diffraction measurements

    International Nuclear Information System (INIS)

    Ferguson, I.F.; Rogerson, A.H.

    1984-01-01

    The program, FIRESTAR, determines the dimensions of a crystallographic unit cell from a set of X-ray powder diffraction measurements corresponding to a set of Bragg reflections, provided that the crystal system applicable is known and the Bragg reflections have been indexed. The program includes a range of possible extrapolation functions, and the data may be weighted. Provision is made for detecting and rejecting a single 'bad' measurement, and then rejecting measurements which lie outside an error limit set in the input data. (orig.)

  7. Analysis of an industrial production suspension of Bacillus lentus subtilisin crystals by powder diffraction: a powerful quality-control tool.

    Science.gov (United States)

    Frankaer, Christian G; Moroz, Olga V; Turkenburg, Johan P; Aspmo, Stein I; Thymark, Majbritt; Friis, Esben P; Stahl, Kenny; Nielsen, Jens E; Wilson, Keith S; Harris, Pernille

    2014-04-01

    A microcrystalline suspension of Bacillus lentus subtilisin (Savinase) produced during industrial large-scale production was analysed by X-ray powder diffraction (XRPD) and X-ray single-crystal diffraction (MX). XRPD established that the bulk microcrystal sample representative of the entire production suspension corresponded to space group P212121, with unit-cell parameters a = 47.65, b = 62.43, c = 75.74 Å, equivalent to those for a known orthorhombic crystal form (PDB entry 1ndq). MX using synchrotron beamlines at the Diamond Light Source with beam dimensions of 20 × 20 µm was subsequently used to study the largest crystals present in the suspension, with diffraction data being collected from two single crystals (∼20 × 20 × 60 µm) to resolutions of 1.40 and 1.57 Å, respectively. Both structures also belonged to space group P2(1)2(1)2(1), but were quite distinct from the dominant form identified by XRPD, with unit-cell parameters a = 53.04, b = 57.55, c = 71.37 Å and a = 52.72, b = 57.13, c = 65.86 Å, respectively, and refined to R = 10.8% and Rfree = 15.5% and to R = 14.1% and Rfree = 18.0%, respectively. They are also different from any of the forms previously reported in the PDB. A controlled crystallization experiment with a highly purified Savinase sample allowed the growth of single crystals of the form identified by XRPD; their structure was solved and refined to a resolution of 1.17 Å with an R of 9.2% and an Rfree of 11.8%. Thus, there are at least three polymorphs present in the production suspension, albeit with the 1ndq-like microcrystals predominating. It is shown how the two techniques can provide invaluable and complementary information for such a production suspension and it is proposed that XRPD provides an excellent quality-control tool for such suspensions.

  8. Ab-initio crystal structure analysis and refinement approaches of oligo p-benzamides based on electron diffraction data

    DEFF Research Database (Denmark)

    Gorelik, Tatiana E; van de Streek, Jacco; Kilbinger, Andreas F M

    2012-01-01

    Ab-initio crystal structure analysis of organic materials from electron diffraction data is presented. The data were collected using the automated electron diffraction tomography (ADT) technique. The structure solution and refinement route is first validated on the basis of the known crystal stru...

  9. Protein crystal growth on board Shenzhou 3: a concerted effort improves crystal diffraction quality and facilitates structure determination

    International Nuclear Information System (INIS)

    Han, Y.; Cang, H.-X.; Zhou, J.-X.; Wang, Y.-P.; Bi, R.-C.; Colelesage, J.; Delbaere, L.T.J.; Nahoum, V.; Shi, R.; Zhou, M.; Zhu, D.-W.; Lin, S.-X.

    2004-01-01

    The crystallization of 16 proteins was carried out using 60 wells on board Shenzhou 3 in 2002. Although the mission was only 7 days, careful and concerted planning at all stages made it possible to obtain crystals of improved quality compared to their ground controls for some of the proteins. Significantly improved resolutions were obtained from diffracted crystals of 4 proteins. A complete data set from a space crystal of the PEP carboxykinase yielded significantly higher resolution (1.46 A vs. 1.87 A), I/sigma (22.4 vs. 15.5), and a lower average temperature factor (29.2 A 2 vs. 42.9 A 2 ) than the best ground-based control crystal. The 3-D structure of the enzyme is well improved with significant ligand density. It has been postulated that the reduced convection and absence of macromolecule sedimentation under microgravity have advantages/benefits for protein crystal growth. Improvements in experimental design for protein crystal growth in microgravity are ongoing

  10. Neutron diffraction study of crystal structures of deuterated glycinium phosphite in paraelectric and ferroelectric phases

    International Nuclear Information System (INIS)

    Machida, Mitsuo; Uchida, Hiroyuki; Ishibashi, Toku; Taniguchi, Hiroki; Komukae, Masaru; Osaka, Toshio; Koyano, Nobumitsu

    2004-01-01

    Crystal structure of deuterated glycinium phosphite was studied in the paraelectric (P) phase at 348 K and in the ferroelectric (F) phase at 223 K by means of the single crystal neutron diffraction. Deuteration rate is estimated to be 0.939 by the least-squares refinement. In the P phase, quasi-one-dimensional hydrogen bond chains are built by mutually linking the DPO 3 2- anions through two different types of hydrogen bonds with the bond angles of 179.2 and 171.6deg. Two independent deuterons within the hydrogen bonds forming the chains are disordered over two sites separated by 0.545 and 0.539A. In the F phase, they order at a position nearly equal to one of two sites related by the disorder in the P phase. With the ordering of the deuterons, the P-O bonds with covalently bonded deuteron elongate, and those without covalently bonded deuteron reduce their lengths to some extend from the values determined in the P phase. Two oxygens involved in the hydrogen bond with the bond angle 179.2deg exhibits especially large displacements in the F phase. This suggests strongly an importance of this hydrogen bond in the polarization appearance and in the ferroelectric transition. Comparison with results of non-deuterated salt indicates that only the hydrogen bonds forming the chains show significant isotope shift. In particular, the hydrogen bond with the bond angle 179.2deg exhibits the most pronounced shift on the angle parameter defined by the angle between the line connecting two sites of disordered proton or deuteron and the line connecting two oxygens involved in the hydrogen bond. (author)

  11. Growth and surface topography of WSe_2 single crystal

    International Nuclear Information System (INIS)

    Dixit, Vijay; Vyas, Chirag; Pataniya, Pratik; Jani, Mihir; Pathak, Vishal; Patel, Abhishek; Pathak, V. M.; Patel, K. D.; Solanki, G. K.

    2016-01-01

    Tungsten Di-Selenide belongs to the family of TMDCs showing their potential applications in the fields of Optoelectronics and PEC solar cells. Here in the present investigation single crystals of WSe_2 were grown by Direct Vapour Transport Technique in a dual zone furnace having temperature difference of 50 K between the two zones. These single crystals were characterized by EDAX which confirms the stiochiometry of the grown crystals. Surface topography of the crystal was studied by optical micrograph showing the left handed spirals on the surface of WSe_2 crystals. Single crystalline nature of the crystals was confirmed by SAED.

  12. Large-scale single-crystal growth of (CH3)2NH2CuCl3 for neutron scattering experiments

    Science.gov (United States)

    Park, Garam; Oh, In-Hwan; Park, J. M. Sungil; Park, Seong-Hun; Hong, Chang Seop; Lee, Kwang-Sei

    2016-05-01

    Neutron scattering studies on low-dimensional quantum spin systems require large-size single-crystals. Single-crystals of (CH3)2NH2CuCl3 showing low-dimensional magnetic behaviors were grown by a slow solvent evaporation method in a two-solvent system at different temperature settings. The best results were obtained for the bilayer solution of methanol and isopropanol with a molar ratio of 2:1 at 35 °C. The quality of the obtained single-crystals was tested by powder and single-crystal X-ray diffraction and single-crystal neutron diffraction. In addition, to confirm structural phase transitions (SPTs), thermal analysis and single-crystal X-ray diffraction at 300 K and 175 K, respectively, were conducted, confirming the presence of a SPT at Tup=288 K on heating and Tdown=285 K on cooling.

  13. Crystallization and preliminary X-ray diffraction analysis of the fructofuranosidase from Schwanniomyces occidentalis

    International Nuclear Information System (INIS)

    Polo, Aitana; Álvaro-Benito, Miguel; Fernández-Lobato, María; Sanz-Aparicio, Julia

    2009-01-01

    The invertase from Schwanniomyces occidentalis has been expressed in Saccharomyces cerevisiae, purified and crystallized. The wild-type enzyme was also purified and crystallized and diffraction data were collected to 2.9 Å resolution. Schwanniomyces occidentalis invertase is an extracellular enzyme that releases β-fructose from the nonreducing termini of various β-d-fructofuranoside substrates. Its ability to produce 6-kestose by transglycosylation makes this enzyme an interesting research target for applications in industrial biotechnology. The enzyme has been expressed in Saccharomyces cerevisiae. Recombinant and wild-type forms, which showed different glycosylation patterns, were crystallized by vapour-diffusion methods. Although crystallization trials were conducted on both forms of the protein, crystals suitable for X-ray crystallographic analyses were only obtained from the wild-type enzyme. The crystals belonged to space group P2 1 2 1 2 1 , with unit-cell parameters a = 105.78, b = 119.49, c = 137.68 Å. A diffraction data set was collected using a synchrotron source. Self-rotation function and sedimentation-velocity experiments suggested that the enzyme was dimeric with twofold symmetry

  14. Neutron diffraction tomography: a unique, 3D inspection technique for crystals using an intensifier TV system

    International Nuclear Information System (INIS)

    Davidson, J.B.; Case, A.L.

    1978-01-01

    The application of phosphor-intensifier-TV techniques to neutron topography and tomography of crystals is described. The older, analogous x-ray topography using wavelengths approximately 1.5A is widely used for surface inspection. However, the crystal must actually be cut in order to see diffraction anomalies beneath the surface. Because 1.5-A thermal neutrons are highly penetrating, much larger and thicker specimens can be used. Also, since neutrons have magnetic moments, they are diffracted by magnetic structures within crystals. In neutron volume topography, the entire crystal or a large part of it is irradiated, and the images obtained are superimposed reflections from the total volume. In neutron tomography (or section topography), a collimated beam irradiates a slice (0.5 to 10 mm) of the crystal. The diffracted image is a tomogram from this part only. A series of tomograms covering the crystal can be taken as the specimen is translated in steps across the narrow beam. Grains, voids, twinning, and other defects from regions down to 1 mm in size can be observed and isolated. Although at present poorer in resolution than the original neutron and film methods, the TV techniques are much faster and, in some cases, permit real-time viewing. Two camera systems are described: a counting camera having a 150 mm 6 Li-ZnS screen for low-intensity reflections which are integrated in a digital memory, and a 300-mm system using analog image storage. Topographs and tomograms of several crystals ranging in size from 4 mm to 80 mm are shown

  15. Thermal shock cracking of GSO single crystal

    International Nuclear Information System (INIS)

    Miyazaki, Noriyuki; Yamamoto, Kazunari; Tamura, Takaharu; Kurashige, Kazuhisa; Ishibashi, Hiroyuki; Susa, Kenzo

    1998-01-01

    The quantitative estimation of the failure stress of a gadolinium orthosilicate (Gd 2 SiO 5 , hereafter abbreviated as GSO) single crystal due to thermal shock was investigated. A cylindrical test specimen was heated in a silicone oil bath, then subjected to thermal shock by pouring room temperature silicone oil. Cracking occurred during cooling. The heat conduction analysis was performed to obtain temperature distribution in a GSO single crystal at cracking, using the surface temperatures measured in the thermal shock cracking test. Then the thermal stress was calculated using temperature profile of the test specimen obtained from the heat conduction analysis. It is found from the results of the thermal stress analysis and the observation of the cracking in test specimens that the thermal shock cracking occurs in a cleavage plane due to the stress normal to the plane. Three-point bending tests were also performed to examine the relationship between the critical stress for thermal shock cracking and the three-point bending strength obtained from small-sized test specimens. (author)

  16. Neutron diffraction investigation of the crystal and molecular structure of the anisotropic superconductor Hg3AsF6

    International Nuclear Information System (INIS)

    Schultz, A.J.; Williams, J.M.; Miro, N.D.; MacDiarmid, A.G.; Heeger, A.J.

    1978-01-01

    The crystal and molecular structure of Hg 3 AsF 6 has been investigated by single-crystal neutron diffraction. This metallic compound crystallizes in the body-centered tetragonal space group I4 1 /amd with cell dimensions of a = 7.549 (5) A and c = 12.390 (9) A. The crystal structure consists of two orthogonal and nonintersecting linear chains of Hg/sup 0.33+/ cations passing through a lattice of octahedral AsF 6 - anions. The intrachain Hg--Hg distance of 2.64 (2) A is derived from planes of diffuse scattering normal to a* and b*. Since the a and b axis lattice constants are not simple multiples of the Hg--Hg intrachain distance, the mercury chains are incommensurate with the tetragonal lattice; hence we have the apparent formula Hg 2 . 86 AsF 6 . These results are in essential agreement with a previously reported x-ray diffraction study. However, from the neutron diffraction data, we have established that the Hg chains are not strictly one-dimensional. The maximum room-temperature deviation from the chain axis is 0.07 (1) A with neighboring chains distorted away from each other. The closest interchain Hg--Hg contact is 3.24 (2) A. Furthermore, analytical data consistently indicate a stoichiometric empirical formula of Hg 3 AsF 6 . These results together with precise density measurements imply that the incommensurate structure is stabilized by anion vacancies, such that there are four formula weights of Hg 2 . 86 (AsF 6 ) 0 . 953 per unit cell. 4 tables, 2 figures

  17. Growth of Cd0.96Zn0.04Te single crystals by vapor phase gas transport method

    Directory of Open Access Journals (Sweden)

    S. H. Tabatabai Yazdi

    2006-03-01

    Full Text Available   Cd0.96Zn0.04Te crystals were grown using vapor phase gas transport method (VPGT. The results show that dendritic crystals with grain size up to 3.5 mm can be grown with this technique. X-ray diffraction and Laue back-reflection patterns show that dendritic crystals are single-phase, whose single crystal grains are randomly oriented with respect to the gas-transport axis. Electrical measurements, carried out using Van der Pauw method, show that the as-grown crystals have resistivity of about 104 Ω cm and n-type conductivity.

  18. Effect of neutron irradiation on single crystal V3Si

    International Nuclear Information System (INIS)

    Viswanathan, R.; Caton, R.; Cox, D.E.; Guha, A.; Sarachik, M.P.; Smith, F.W.; Testardi, L.R.

    1977-01-01

    We We have investigated the effect of successive neutron irradiation up to a fluence of approximately 2 x 10 19 n/cm 2 , by measurements of heat capacity, susceptibility, resistivity, acoustic velocity and neutron diffraction in a single crystal V 3 Si. We find that for low level doses (phi t greater than or equal to 3.5 x 10 18 n/cm 2 ) (a) the structural transformation is very sensitive, whereas the suerconducting transition temperature, T/sub c/, is hardly affected, and (b) except for low temperature heat capacity, most of the other measurements show very little change. For the highest fluence of 2 x 10 19 n/cm 2 used to date, the T/sub c/ dropped to 7.5 K with large changes in the linear heat capacity coefficient, magnetic susceptibility and sound velocity. These results are discussed briefly in this paper

  19. Neutron radiation damage in NbO single crystals

    International Nuclear Information System (INIS)

    Onozuka, T.; Koiwa, M.; Ishikawa, Y.; Yamaguchi, S.; Hirabayashi, M.

    1977-01-01

    The effect of neutron irradiation and subsequent recovery has been studied for Nb0 single crystals of a defective NaCl structure containing 25% vacancies of niobium and oxygen. A very large increase (about 1%) in the lattice constant is observed after irradiation of 1.5 x 10 19 and 1 x 10 20 nvt (> 1 MeV). From the intensity measurements of x-ray and neutron diffraction, it is revealed that the knock-on atoms fill preferentially their respective vacant sites; Nb atoms occupy Nb-vacancies, and 0 atoms occupy 0-vacancies with nearly the same probabilities; 0.53 for 1.5 x 10 19 nvt. The mean threshold energy for displacement is estimated to be about 3 eV. (author)

  20. Magnetic order of Nd5Pb3 single crystals

    Science.gov (United States)

    Yan, J.-Q.; Ochi, M.; Cao, H. B.; Saparov, B.; Cheng, J.-G.; Uwatoko, Y.; Arita, R.; Sales, B. C.; Mandrus, D. G.

    2018-04-01

    We report millimeter-sized Nd5Pb3 single crystals grown out of a Nd-Co flux. We experimentally study the magnetic order of Nd5Pb3 single crystals by measuring the anisotropic magnetic properties, electrical resistivity under high pressure up to 8 GPa, specific heat, and neutron single crystal diffraction. Two successive magnetic orders are observed at T N1  =  44 K and T N2  =  8 K. The magnetic cells can be described with a propagation vector k=(0.5, 0, 0) . Cooling below T N1, Nd1 and Nd3 order forming ferromagnetic stripes along the b-axis, and the ferromagnetic stripes are coupled antiferromagnetically along the a-axis for the k=(0.5, 0, 0) magnetic domain. Cooling below T N2, Nd2 orders antiferromagnetically to nearby Nd3 ions. All ordered moments align along the crystallographic c-axis. The magnetic order at T N1 is accompanied by a quick drop of electrical resistivity upon cooling and a lambda-type anomaly in the temperature dependence of specific heat. At T N2, no anomaly was observed in electrical resistivity but there is a weak feature in specific heat. The resistivity measurements under hydrostatic pressures up to 8 GPa suggest a possible phase transition around 6 GPa. Our first-principles band structure calculations show that Nd5Pb3 has the same electronic structure as does Y5Si3 which has been reported to be a one-dimensional electride with anionic electrons that do not belong to any atom. Our study suggests that R 5Pb3 (R  =  rare earth) can be a materials playground for the study of magnetic electrides. This deserves further study after experimental confirmation of the presence of anionic electrons.

  1. Studies of the surface structures of molecular crystals and of adsorbed molecular monolayers on the (111) crystal faces of platinum and silver by low-energy electron diffraction

    International Nuclear Information System (INIS)

    Firment, L.E.

    1977-01-01

    The structures of molecular crystal surfaces were investigated for the first time by the use of low-energy electron diffraction (LEED). The experimental results from a variety of molecular crystals were examined and compared as a first step towards understanding the properties of these surfaces on a microscopic level. The method of sample preparation employed, vapor deposition onto metal single-crystal substrates at low temperatures in ultrahigh vacuum, allowed concurrent study of the structures of adsorbed monolayers on metal surfaces and of the growth processes of molecular films on metal substrates. The systems investigated were ice, ammonia, naphthalene, benzene, the n-paraffins (C 3 to C 8 ), cyclohexane, trioxane, acetic acid, propionic acid, methanol, and methylamine adsorbed and condensed on both Pt(111) and Ag(111) surfaces. Electron-beam-induced damage of the molecular surfaces was observed after electron exposures of 10 -4 A sec cm -2 at 20 eV. Aromatic molecular crystal samples were more resistant to damage than samples of saturated molecules. The quality and orientation of the grown molecular crystal films were influenced by substrate preparation and growth conditions. Forty ordered monolayer structures were observed. 110 figures, 22 tables, 162 references

  2. Phase transitions in A4Li(HSO4)3(SO4); A = Rb, K: Single crystal X ...

    Indian Academy of Sciences (India)

    Unknown

    Single crystal studies on RLHS at room temperature (293 K) reported earlier5 showed that the crystals are optically laevorotatory and belong to the enantiomorphous space group P41. However, an analysis of the diffraction data based on the value of enantio- morph polarity parameter during refinement suggested that the ...

  3. Growth of single crystals of BaFe12O19 by solid state crystal growth

    Science.gov (United States)

    Fisher, John G.; Sun, Hengyang; Kook, Young-Geun; Kim, Joon-Seong; Le, Phan Gia

    2016-10-01

    Single crystals of BaFe12O19 are grown for the first time by solid state crystal growth. Seed crystals of BaFe12O19 are buried in BaFe12O19+1 wt% BaCO3 powder, which are then pressed into pellets containing the seed crystals. During sintering, single crystals of BaFe12O19 up to ∼130 μm thick in the c-axis direction grow on the seed crystals by consuming grains from the surrounding polycrystalline matrix. Scanning electron microscopy-energy dispersive spectroscopy analysis shows that the single crystal and the surrounding polycrystalline matrix have the same chemical composition. Micro-Raman scattering shows the single crystal to have the BaFe12O19 structure. The optimum growth temperature is found to be 1200 °C. The single crystal growth behavior is explained using the mixed control theory of grain growth.

  4. Determining the diffraction properties of a cylindrically bent KAP(001) crystal from 1 to 5 keV

    Energy Technology Data Exchange (ETDEWEB)

    Haugh, Michael [National Security Technologies, LLC. (NSTec), Mercury, NV (United States); Lee, Joshua [National Security Technologies, LLC. (NSTec), Mercury, NV (United States); Jacoby, Kenneth [National Security Technologies, LLC. (NSTec), Mercury, NV (United States); Christensen, C. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Loisel, G. [National Security Technologies, LLC. (NSTec), Mercury, NV (United States), Livermore Operations

    2015-08-31

    Various crystals are used for the dispersive component of X-ray spectrometers. The crystals are usually bent to meet the desired measurement needs, such as focusing. The bending can change the crystal diffraction properties, thus altering the spectrometer throughput and resolving power. This work concerns measuring the diffraction properties of a potassium acid phthalate (001) [KAP(001)] crystal bent into a circular cylinder segment. The measurement methods using a diode source and a synchrotron source are described. The multi-lamellar model for calculating the diffraction properties of a bent crystal is described. The measurement results are compared to the multi-lamellar model and show qualitative agreement. The measurements show how to make the multi-lamellar calculations a useful estimate. A method is given to make useful estimates of the diffraction properties of the KAP(001) crystal bent into a circular cylinder segment.

  5. Crystal structure solution of hydrides containing natEu from neutron powder diffraction data

    International Nuclear Information System (INIS)

    Kohlmann, H.

    1999-01-01

    Complete text of publication follows. The location of hydrogen in crystal structures of metal hydrides usually requires neutron diffraction data. Some elements, however, show excessively high absorption cross sections, σ a , for neutrons, thus making this technique seemingly impractical. Therefore no complete, refined crystal structure data of europium hydrides (σ a ( nat Eu) = .4530 barns at λ = 179.8 pm [1]) have been reported so far. It is shown that the absorption can be reduced to a value reasonable for neutron diffraction experiments by taking advantage of the wavelength dependence of σ a combined with the use of annular samples at advanced diffractometers. Neutron powder diffraction data on several nat Eu containing deuterides suitable for the ab initio crystal structure solution and refinement have been taken at D20 and D4 (ILL, Grenoble). The crystal chemistry of these europium hydrides, among them the two new compounds EuMg 2 H 6 and EuMgH 4 [2], is discussed. (author) [1] V.F. Sears, Neutron News 1992, 3, 26-37.; [2] H. Kohlmann, F. Gingl, T. Hansen, K. Yvon, Angew. Chem. Int. Ed. Eng. 1999, 38, accepted

  6. In situ high-pressure measurement of crystal solubility by using neutron diffraction

    Science.gov (United States)

    Chen, Ji; Hu, Qiwei; Fang, Leiming; He, Duanwei; Chen, Xiping; Xie, Lei; Chen, Bo; Li, Xin; Ni, Xiaolin; Fan, Cong; Liang, Akun

    2018-05-01

    Crystal solubility is one of the most important thermo-physical properties and plays a key role in industrial applications, fundamental science, and geoscientific research. However, high-pressure in situ measurements of crystal solubility remain very challenging. Here, we present a method involving high-pressure neutron diffraction for making high-precision in situ measurements of crystal solubility as a function of pressure over a wide range of pressures. For these experiments, we designed a piston-cylinder cell with a large chamber volume for high-pressure neutron diffraction. The solution pressures are continuously monitored in situ based on the equation of state of the sample crystal. The solubility at a high pressure can be obtained by applying a Rietveld quantitative multiphase analysis. To evaluate the proposed method, we measured the high-pressure solubility of NaCl in water up to 610 MPa. At a low pressure, the results are consistent with the previous results measured ex situ. At a higher pressure, more reliable data could be provided by using an in situ high-pressure neutron diffraction method.

  7. Crystal optimization and preliminary diffraction data analysis of the SCAN domain of Zfp206

    International Nuclear Information System (INIS)

    Liang, Yu; Choo, Siew Hua; Rossbach, Michael; Baburajendran, Nithya; Palasingam, Paaventhan; Kolatkar, Prasanna R

    2012-01-01

    Crystals of the SCAN domain of Zfp206 are tetragonal, belonging to space group I422 with unit-cell parameters a = 67.57, c = 87.54 Å and one molecule in the asymmetric unit, and diffract to 1.85 Å resolution. Zfp206 (also named Zscan10) is a transcription factor that plays an important role in maintaining the pluripotent state of embryonic stem cells. Zfp206 is a member of the SCAN-domain family of C 2 H 2 zinc-finger transcription factors. The SCAN domain is a highly conserved motif of 84 residues which mediates the self-association of and heterodimerization between SCAN-domain family transcription factors. The SCAN domain may therefore be the key to the selective oligomerization of and may combinatorially enhance the regulatory versatility of C 2 H 2 zinc fingers. This paper describes crystallization attempts with the SCAN domain of Zfp206 (Zfp206SCAN) and optimization strategies to obtain diffraction-quality crystals. The best diffracting crystal was grown in a solution consisting of 0.3 M ammonium sulfate, 0.1 M Tris–HCl pH 8.6, 25% PEG 3350, 0.1 M ethylenediaminetetraacetic acid disodium salt dehydrate (EDTA) using the hanging-drop vapour-diffusion technique. Optimized crystals diffracted to 1.85 Å resolution and belonged to space group I422, with unit-cell parameters a = 67.57, c = 87.54 Å. A Matthews analysis indicated the presence of one Zfp206SCAN molecule per asymmetric unit

  8. Corelli: Efficient single crystal diffraction with elastic discrimination

    Indian Academy of Sciences (India)

    treme field response of many emerging phenomena of great interest. .... development at SNS, i.e., facing the high-resolution water moderator [17], a disk .... increasingly less effective and inelastic contamination finally leads to the deviation.

  9. Zinc (tris) thiourea sulphate (ZTS): A single crystal neutron diffraction ...

    Indian Academy of Sciences (India)

    organic crys- tal which is used for electro-optical (EO) applications and frequency doubling ... P U Sastry et al. Table 1. Bond distances (in Å units) in ZTS. Zn–O(1) 1.984(6) S(1)–O(1) 1.463(7) H(2)–O(3) 1.987(8) H(7)–O(4) 1.843(7). Zn–S(2) 2.330(4) ...

  10. Crystal structure analysis of LaMnO_3 with x-ray diffraction technique using the Rietveld method

    International Nuclear Information System (INIS)

    Engkir Sukirman; Wisnu Ari Adi; Yustinus Purwamargapratala

    2010-01-01

    Crystal structure analysis of LaMnO_3 using the Rietveld method has been carried out. The LaMnO_3 sample was synthesized with high energy mechanical milling from the raw materials of La_2O_3 and MnO_2 with the appropriate mol ratio. Milling were performed for 10 hours, pelletized and hereinafter sintered at 1350 °C for 6 hours. The sample characterizations covered the crystal structure and electric-magnetic properties of the materials by X-ray diffraction technique using the Rietveld method and the four point probe, respectively. The Rietveld refinement results based on the X-rays diffraction data indicate that the sample of LaMnO_3 is single phase with the crystal system: orthorhombic, the space group: Pnma No. 62 and the lattice parameters: a = 55.4405(9) Å; b = 7.717(1) Å dan c = 5.537(1) Å. The material owns Magnetic Resonance (MR) respond of 7 %, the mean value of crystallite size, D = 17 nm and lattice strain, e = - 0.5 %. So, the material go through a compressive strain, and according to the Nanda's strain model, it becomes a type G antiferromagnetic insulator. Because the insulator properties of the material does not change although being hit by the external magnetic field, hence the MR respond is only caused by the order of electron spin. Therefore at room temperature, LaMnO_3_._0 just exhibits a small MR respond. (author)

  11. Crystallization and preliminary X-ray diffraction analysis of the putative aldose 1-epimerase YeaD from Escherichia coli

    International Nuclear Information System (INIS)

    You, Weijie; Qiu, Xiaoting; Zhang, Yujie; Ma, Jinming; Gao, Yongxiang; Zhang, Xiao; Niu, Liwen; Teng, Maikun

    2010-01-01

    The putative aldose 1-epimerase YeaD from Escherichia coli was crystallized and diffraction data were collected to a resolution of 1.9 Å. Escherichia coli YeaD (ecYeaD) is suggested to be a member of the galactose mutarotase-like superfamily. Galactose mutarotase is an enzyme that converts α-galactose to β-galactose. The known structures of these galactose mutarotase-like proteins are similar to those of galactose mutarotases, with the catalytic residues being conserved, but there are some differences between them in the substrate-binding pocket. In order to reveal the specificity of ecYeaD, a three-dimensional structure is essential. Full-length ecYeaD with an additional 6×His tag at the C-terminus was crystallized by the hanging-drop vapour-diffusion method using polyethylene glycol 4000 as a precipitant at 283 K. An X-ray diffraction data set was collected to a resolution of 1.9 Å from a single flash-cooled crystal that belonged to space group P2 1 2 1 2 1

  12. Dynamic Diffraction Studies on the Crystallization, Phase Transformation, and Activation Energies in Anodized Titania Nanotubes.

    Science.gov (United States)

    Albetran, Hani; Vega, Victor; Prida, Victor M; Low, It-Meng

    2018-02-23

    The influence of calcination time on the phase transformation and crystallization kinetics of anodized titania nanotube arrays was studied using in-situ isothermal and non-isothermal synchrotron radiation diffraction from room temperature to 900 °C. Anatase first crystallized at 400 °C, while rutile crystallized at 550 °C. Isothermal heating of the anodized titania nanotubes by an increase in the calcination time at 400, 450, 500, 550, 600, and 650 °C resulted in a slight reduction in anatase abundance, but an increase in the abundance of rutile because of an anatase-to-rutile transformation. The Avrami equation was used to model the titania crystallization mechanism and the Arrhenius equation was used to estimate the activation energies of the titania phase transformation. Activation energies of 22 (10) kJ/mol for the titanium-to-anatase transformation, and 207 (17) kJ/mol for the anatase-to-rutile transformation were estimated.

  13. Crystallization and preliminary X-ray diffraction studies of Murraya koenigii trypsin inhibitor

    Energy Technology Data Exchange (ETDEWEB)

    Shee, Chandan [Department of Biotechnology, Indian Institute of Technology Roorkee, Roorkee 247 667 (India); Singh, Tej P. [Department of Biophysics, All India Institute of Medical Sciences, New Delhi 100 029 (India); Kumar, Pravindra, E-mail: kumarfbs@iitr.ernet.in; Sharma, Ashwani K., E-mail: kumarfbs@iitr.ernet.in [Department of Biotechnology, Indian Institute of Technology Roorkee, Roorkee 247 667 (India)

    2007-04-01

    A Kunitz-type trypsin inhibitor purified from the seeds of Murraya koenigii has been crystallized by the sitting-drop vapour-diffusion method using PEG 8000 as the precipitating agent. A Kunitz-type trypsin inhibitor purified from the seeds of Murraya koenigii has been crystallized by the sitting-drop vapour-diffusion method using PEG 8000 as the precipitating agent. The crystals belong to the tetragonal space group P4{sub 3}2{sub 1}2, with unit-cell parameters a = b = 75.8, c = 150.9 Å. The crystals contain two molecules in the asymmetric unit with a V{sub M} value of 2.5 Å{sup 3} Da{sup −1}. Diffraction was observed to 2.65 Å resolution and a complete data set was collected to 2.9 Å resolution.

  14. Computer simulations of X-ray six-beam diffraction in a perfect silicon crystal. I

    Czech Academy of Sciences Publication Activity Database

    Kohn, V.G.; Khikhlukha, Danila

    2016-01-01

    Roč. 72, May (2016), s. 349-356 ISSN 2053-2733 R&D Projects: GA MŠk EF15_008/0000162; GA MŠk ED1.1.00/02.0061 Grant - others:ELI Beamlines(XE) CZ.02.1.01/0.0/0.0/15_008/0000162; ELI Beamlines(XE) CZ.1.05/1.1.00/02.0061 Institutional support: RVO:68378271 Keywords : X-ray diffraction * silicon crystal * six-beam diffraction * section topography * computer simulations Subject RIV: BL - Plasma and Gas Discharge Physics OBOR OECD: Fluids and plasma physics (including surface physics) Impact factor: 5.725, year: 2016

  15. Growth and characterization of 2-Methylimidazolium D-tartrate single crystal

    Science.gov (United States)

    Srinivasan, T. P.; Anandhi, S.; Gopalakrishnan, R.

    2011-03-01

    Single crystal of 2-Methylimidazolium D-tartrate (2MImdT; C8N2O6H12) has been grown by slow evaporation solution growth technique at room temperature using mixed solvents of ethanol and deionized water. Single crystal X-ray diffraction study confirms that 2-Methylimidazolium D-tartrate belongs to monoclinic crystal system with non-centrosymmetric space group P21. The Fourier transform infrared spectrum of 2-Methylimidazolium D-tartrate reveals the presence of methyl and carboxyl functional groups in the compound. The mechanical properties of 2MImdT crystal were studied. The theoretical factor group analysis predicts 168 optical modes in the title compound. The dielectric behavior of 2MImdT crystals was studied at different frequencies and temperatures. Decomposition and melting point of 2MImdT were found using thermal measurements. SHG behavior of the title compound was demonstrated using Q-switched Nd:YAG laser.

  16. Investigations of morphological changes during annealing of polyethylene single crystals

    NARCIS (Netherlands)

    Tian, M.; Loos, J.

    2001-01-01

    The morphological evolution of isolated individual single crystals deposited on solid substrates was investigated during annealing experiments using in situ and ex situ atomic force microscopy techniques. The crystal morphology changed during annealing at temperatures slightly above the original

  17. Single Crystals of Organolead Halide Perovskites: Growth, Characterization, and Applications

    KAUST Repository

    Peng, Wei

    2017-01-01

    Despite their outstanding charge transport characteristics, organolead halide perovskite single crystals grown by hitherto reported crystallization methods are not suitable for most optoelectronic devices due to their small aspect ratios

  18. High-quality single crystals for neutron experiments

    Indian Academy of Sciences (India)

    studies and our collaborative research projects with other UK and international groups will be discussed. Keywords. Crystal growth; floating zone method; neutron scattering. ... of single crystals of new materials is a highly competitive business.

  19. Growth and characterization of nonlinear optical single crystals: bis ...

    Indian Academy of Sciences (India)

    Administrator

    molecules have received great attention for NLO applica- tions. However ... Figure 3. Single crystals of bis(cyclohexylammonium) terephthalate (crystal a) and cyclohexylammo- .... from ground state to higher energy states.17 Optical window ...

  20. Reversible Single-Crystal-to-Single-Crystal Structural Transformation in a Mixed-Ligand 2D Layered Metal-Organic Framework: Structural Characterization and Sorption Study

    Directory of Open Access Journals (Sweden)

    Chih-Chieh Wang

    2017-12-01

    Full Text Available A 3D supramolecular network, [Cd(bipy(C4O4(H2O2]·3H2O (1 (bipy = 4,4′-bipyridine and C4O42− = dianion of H2C4O4, constructed by mixed-ligand two-dimensional (2D metal-organic frameworks (MOFs has been reported and structurally determined by the single-crystal X-ray diffraction method and characterized by other physicochemical methods. In 1, the C4O42− and bipy both act as bridging ligands connecting the Cd(II ions to form a 2D layered MOF, which are then extended to a 3D supramolecular network via the mutually parallel and interpenetrating arrangements among the 2D-layered MOFs. Compound 1 shows a two-step dehydration process with weight losses of 11.0% and 7.3%, corresponding to the weight-loss of three guest and two coordinated water molecules, respectively, and exhibits an interesting reversible single-crystal-to-single-crystal (SCSC structural transformation upon de-hydration and re-hydration for guest water molecules. The SCSC structural transformation have been demonstrated and monitored by single-crystal and X-ray powder diffraction, and thermogravimetic analysis studies.

  1. Synthesis and photocatalytic activity of mesoporous – (001) facets TiO_2 single crystals

    International Nuclear Information System (INIS)

    Dong, Yeshuo; Fei, Xuening; Zhou, Yongzhu

    2017-01-01

    Highlights: • The (001) facets of TiO_2 single crystals with mesoporous structure. • The (010) and (100) facets of TiO_2 single crystals were covered by the flower – shaped TiO_2 crystals. • This special structure could promote charge separation and provide more active sites, which will lead to a substantial increase in photocatalytic activity. - Abstract: In this work, the mesoporous – (001) facets TiO_2 single crystals have been successfully synthesized through a two-step solvothermal route without any template. Their structure and morphology were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible (UV–vis) diffuse reflectance spectroscopy and energy dispersive X-ray spectrometer (EDX). Based on the different characteristics and atomic arrangements on each facet of anatase TiO_2 single crystals, we synthesized these mesoporous – (001) facets TiO_2 single crystals by controlling the interaction characteristics of hydrofluoric acid (HF) and isopropanol (i-PrOH) on the crystal facets. It can been seen that the (001) facets of these as-synthesized TiO_2 single crystals have a clear mesoporous structure through the SEM images and BET methods. Moreover, the other four facets were covered by the flower – shaped TiO_2 crystals with the generation of the mesoporous – (001) facets. This special and interesting morphology could promote charge separation and provide more active sites, which will lead to a substantial increase in photocatalytic activity. Moreover, it is more intuitive to reflect that the different crystal facets possess the different properties due to their atomic arrangement. Besides, according to the different synthetic routes, we proposed and discussed a plausible synthesis mechanism of these mesoporous – (001) facets TiO_2 single crystals.

  2. Growth and characterization of unidirectional benzil single crystal for photonic applications

    Science.gov (United States)

    Saranraj, A.; Thirupathy, J.; Dhas, S. Sahaya Jude; Jose, M.; Vinitha, G.; Dhas, S. A. Martin Britto

    2018-06-01

    Organic nonlinear optical benzil single crystal of fine quality with the dimensions of 168 × 14 mm2 was successfully grown in (100) plane from saturated solution by unidirectional SR method. The structural identity of the grown crystal was confirmed by powder XRD. High-resolution X-ray diffraction analysis indicates the crystalline perfection of the grown benzil crystal. The optical analysis was carried out by UV-visible spectroscopy which shows that the benzil crystal's cut off wavelength is 437 nm. The dielectric constant and dielectric loss of benzil crystal are found to be very much depending upon temperature and frequency. Ferroelectric nature of grown crystal was identified by P- E hysteresis analysis and to find the values of spontaneous polarization and coercive field. The laser damage threshold energy was studied with the help of Nd:YAG laser. The presence of third harmonic generation was identified by z-scan techniques.

  3. Purification, crystallization and preliminary X-ray diffraction analysis of human Gadd45γ

    International Nuclear Information System (INIS)

    Zhang, Wenzheng; Zhao, Mingzhuo; Li, Jianhui; Li, Xuemei; Zeng, ZongHao; Rao, Zihe

    2008-01-01

    The human Gadd45γ protein has been crystallized as a prelude towards determination of its three-dimensional structure by X-ray crystallography. Gadd45, MyD118 and CR6 (also termed Gadd45α, Gadd45β and Gadd45γ, respectively) comprise a family of proteins that play important roles in negative growth control, maintenance of genomic stability, DNA repair, cell-cycle control and apoptosis. Recombinant human Gadd45γ and its selenomethionine derivative were expressed in an Escherichia coli expression system and purified; they were then crystallized using the hanging-drop vapour-diffusion method. Diffraction-quality crystals were grown at 291 K using PEG 3350 as precipitant. Using synchrotron radiation, the best diffraction data were collected to 2.3 Å resolution for native crystals at 100 K; selenomethionyl derivative data were collected to 3.3 Å resolution. All the crystals belonged to space group I2 1 3, with approximate unit-cell parameters a = b = c = 126 Å

  4. The incidence angle influence on the structure of secondary-emission characteristics of single crystals

    International Nuclear Information System (INIS)

    Gasanov, E.R.; Aliyev, B.Z.

    2012-01-01

    Full text : The dependences of Wand MO single crystals in different atom planes have been studied in this work. It is revealed that maximums are added to each dependency and also minimums of first and second degree. This fact is explained by diffraction dynamic theory. It is established that electron diffraction oriented not perpendicularly to crystal surface is the reason of appearance of second order structure on studied secondary-emission characteristics. In the present work being the continuation and development of SEE investigations of high-melting metal single crystals begun earlier by authors, the structure dependence of SEE main characteristics of angle has been studied. This angle has been chosen because as it is mentioned before the bad repeatability in different experiments for it is observed

  5. Electron diffraction of CBr{sub 4} in superfluid helium droplets: A step towards single molecule diffraction

    Energy Technology Data Exchange (ETDEWEB)

    He, Yunteng; Zhang, Jie; Kong, Wei, E-mail: wei.kong@oregonstate.edu [Department of Chemistry, Oregon State University, Corvallis, Oregon 97331-4003 (United States)

    2016-07-21

    We demonstrate the practicality of electron diffraction of single molecules inside superfluid helium droplets using CBr{sub 4} as a testing case. By reducing the background from pure undoped droplets via multiple doping, with small corrections for dimers and trimers, clearly resolved diffraction rings of CBr{sub 4} similar to those of gas phase molecules can be observed. The experimental data from CBr{sub 4} doped droplets are in agreement with both theoretical calculations and with experimental results of gaseous species. The abundance of monomers and clusters in the droplet beam also qualitatively agrees with the Poisson statistics. Possible extensions of this approach to macromolecular ions will also be discussed. This result marks the first step in building a molecular goniometer using superfluid helium droplet cooling and field induced orientation. The superior cooling effect of helium droplets is ideal for field induced orientation, but the diffraction background from helium is a concern. This work addresses this background issue and identifies a possible solution. Accumulation of diffraction images only becomes meaningful when all images are produced from molecules oriented in the same direction, and hence a molecular goniometer is a crucial technology for serial diffraction of single molecules.

  6. Solar cell structure incorporating a novel single crystal silicon material

    Science.gov (United States)

    Pankove, Jacques I.; Wu, Chung P.

    1983-01-01

    A novel hydrogen rich single crystal silicon material having a band gap energy greater than 1.1 eV can be fabricated by forming an amorphous region of graded crystallinity in a body of single crystalline silicon and thereafter contacting the region with atomic hydrogen followed by pulsed laser annealing at a sufficient power and for a sufficient duration to recrystallize the region into single crystal silicon without out-gassing the hydrogen. The new material can be used to fabricate semiconductor devices such as single crystal silicon solar cells with surface window regions having a greater band gap energy than that of single crystal silicon without hydrogen.

  7. Time-dependent Bragg diffraction and short-pulse reflection by one-dimensional photonic crystals

    International Nuclear Information System (INIS)

    André, Jean-Michel; Jonnard, Philippe

    2015-01-01

    The time-dependence of the Bragg diffraction by one-dimensional photonic crystals and its influence on the short pulse reflection are studied in the framework of the coupled-wave theory. The indicial response of the photonic crystal is calculated and it appears that it presents a time-delay effect with a transient time conditioned by the extinction length. A numerical simulation is presented for a Bragg mirror in the x-ray domain and a pulse envelope modelled by a sine-squared shape. The potential consequences of the time-delay effect in time-dependent optics of short-pulses are emphasized. (paper)

  8. X-ray diffraction in laser-irradiated epsomite crystals grown in presence of borax

    International Nuclear Information System (INIS)

    Zaitseva, E.V.; Portnov, V.N.; Faddeev, M.A.; Chuprunov, E.V.

    1997-01-01

    Relative changes in the intensities ΔI/I of the (220) and (440) X-ray diffraction reflection during laser irradiation of epsomite (MgSO 2 ·7H 2 O) crystals grown from an aqueous solution in the presence of borax (Na 2 B 4 O 7 ·10H 2 O) were measured using the CoK α , CuK α , MoK α radiations. The intensities measured depend on the real crystal structure dependent on the borax content in the solution. The dependence of ΔI/I is studied as a function of borax in the solution and X-ray-radiation wavelength

  9. Hydroniumjarosite, (H.sub.3./sub.O).sup.+./sup.Fe.sub.3./sub.(SO.sub.4./sub.).sub.2./sub.(OH).sub.6./sub., from Cerros Pintados, Chile: single-crystal X-ray diffraction and vibrational spectroscopic study

    Czech Academy of Sciences Publication Activity Database

    Plášil, Jakub; Škoda, R.; Fejfarová, Karla; Čejka, J.; Kasatkin, A.V.; Dušek, Michal; Talla, D.; Lapčák, L.; Machovič, V.; Dini, M.

    2014-01-01

    Roč. 78, č. 3 (2014), s. 535-547 ISSN 0026-461X R&D Projects: GA ČR GP13-31276P Grant - others:AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : hydroniumjarosite * H3O + * crystal structure * vibrational spectroscopy * X-ray diffraction Subject RIV: DB - Geology ; Mineralogy Impact factor: 2.026, year: 2014

  10. Cyclic deformation of Nb single crystals

    International Nuclear Information System (INIS)

    Guiu, F.; Anglada, M.

    1982-01-01

    The temperature and strain-rate dependence of the cyclic flow stress of Nb single crystals with two different axial orientations has been studied at temperatures between 175 and 350 K. This dependence is found to be independent of the crystal orientation when the internal stresses are taken into account, and the results are discussed in terms of the theory of thermally activated dislocation glide. A transition temperature can be identified at about 250 K which separates two regions with different thermally activated deformation behaviour. Above this transition temperature the strain rate can be described by a stress power law, and the activation energy can be represented by a logarithmic function of the stress, as in Escaig's model of screw dislocation mobility. In the temperature range 170 to 250 K the results are also in agreement with the more recent model proposed by Seeger. The large experimental errors inherent in the values of activation enthalpy at low stresses are emphasized and taken into account in the discussion of the results. It is suggested that either impurity-kink interactions or the flexibility of the screw dislocations are responsible for the trend towards the high values of activation enthalpy measured at the low stresses. (author)

  11. High-Resolution Single-Grain Diffraction of Polycrystalline Materials

    DEFF Research Database (Denmark)

    Lienert, Ulrich; Ribárik, Gábor; Ungar, Tamas

    2017-01-01

    . The microstructure usually influences the materials properties critically. It has been demonstrated that, by using high-energy synchrotron radiation, diffraction peaks off individual grains can be recorded in-situ during processing. Important information such as the orientation, average strain, and size...... of individual grains can be obtained, even if the peak shapes are commonly not analyzed. However, it is also well-known that the shape of diffraction peaks, if observed with sufficient resolution, contains significant information about the microstructure. While the intensity distribution in reciprocal space...... of a perfect lattice consists of delta functions located at the reciprocal lattice points, defects induce characteristic peak broadening. In order to exploit the wealth of microstructural information contained in broadened diffraction peaks, the intensity distribution has to be characterized in all three...

  12. Surface structures of normal paraffins and cyclohexane monolayers and thin crystals grown on the (111) crystal face of platinum. A low-energy electron diffraction study

    International Nuclear Information System (INIS)

    Firment, L.E.; Somorjai, G.A.

    1977-01-01

    The surfaces of the normal paraffins (C 3 --C 8 ) and cyclohexane have been studied using low-energy electron diffraction (LEED). The samples were prepared by vapor deposition on the (111) face of a platinum single crystal in ultrahigh vacuum, and were studied both as thick films and as adsorbed monolayers. These molecules form ordered monolayers on the clean metal surface in the temperature range 100--220 K and at a vapor flux corresponding to 10 -7 Torr. In the adsorbed monolayers of the normal paraffins (C 4 --C 8 ), the molecules lie with their chain axes parallel to the Pt surface and Pt[110]. The paraffin monolayer structures undergo order--disorder transitions as a function of temperature. Multilayers condensed upon the ordered monolayers maintained the same orientation and packing as found in the monolayers. The surface structures of the growing organic crystals do not corresond to planes in their reported bulk crystal structures and are evidence for epitaxial growth of pseudomorphic crystal forms. Multilayers of n-octane and n-heptane condensed upon disordered monolayers have also grown with the (001) plane of the triclinic bulk crystal structures parallel to the surface. n-Butane has three monolayer structures on Pt(111) and one of the three is maintained during growth of the crystal. Cyclohexane forms an ordered monolayer, upon which a multilayer of cyclohexane grows exhibiting the (001) surface orientation of the monoclinic bulk crystal structure. Surface structures of saturated hydrocarbons are found to be very susceptible to electron beam induced damage. Surface charging interferes with LEED only at sample thicknesses greater than 200 A

  13. Investigations on the nucleation kinetics of γ-glycine single crystal

    International Nuclear Information System (INIS)

    Yogambal, C.; Rajan Babu, D.; Ezhil Vizhi, R.

    2014-01-01

    Single crystals of γ-glycine were grown by slow evaporation technique. The crystalline system was confirmed by single crystal X-ray diffraction analysis. The optical absorption study has shown that the grown crystal possesses lower cut-off wavelength. Solubility and metastable zone width were estimated for different temperatures. The induction period of title compound was determined by varying the temperature and concentration. Nucleation parameters such as Gibbs volume free energy change (ΔG v ), interfacial tension (γ), critical free energy change of the nucleus (ΔG ⁎ ), nucleation rate (J), number of molecules in the critical nucleus (i ⁎ ) have been calculated for the aqueous solution grown γ-glycine single crystals. The second harmonic generation (SHG) of γ-glycine was confirmed by Q-switched Nd:YAG laser technique

  14. Highly efficient single-pass sum frequency generation by cascaded nonlinear crystals

    DEFF Research Database (Denmark)

    Hansen, Anders Kragh; Andersen, Peter E.; Jensen, Ole Bjarlin

    2015-01-01

    , despite differences in the phase relations of the involved fields. An unprecedented 5.5 W of continuous-wave diffraction-limited green light is generated from the single-pass sum frequency mixing of two diode lasers in two periodically poled nonlinear crystals (conversion efficiency 50%). The technique......The cascading of nonlinear crystals has been established as a simple method to greatly increase the conversion efficiency of single-pass second-harmonic generation compared to a single-crystal scheme. Here, we show for the first time that the technique can be extended to sum frequency generation...... is generally applicable and can be applied to any combination of fundamental wavelengths and nonlinear crystals....

  15. Growth Aspects, Structural and Optical Properties of 2-aminopyridinium 2,4 Dinitrophenolate Single Crystal

    Directory of Open Access Journals (Sweden)

    S. Reena Devi

    2017-06-01

    Full Text Available Organic single crystal of 2-aminopyridinium 2,4-dinitrophenolate single crystal was grown by slow evaporation technique. The cell parameters and space group (P were determined from single X-ray diffraction analysis. HRXRD studies ascertained the crystalline quality. UV-Visible and PL spectral studies revealed the emission in red region, transparency (75% cutoff wavelength around 440 nm respectively. The laser damage threshold of grown crystal was estimated by using Nd:YAG laser beam and these results were mutually related with specific heat capacity of the grown crystal. The third-order nonlinear optical parameters were estimated by Z-scan technique which is useful for optical applications.

  16. Integrated intensities and flipping ratios in neutron diffraction by perfect magnetic crystals

    International Nuclear Information System (INIS)

    Guigay, J.P.; Schlenker, M.

    1979-01-01

    A theoretical study of neutron diffraction by perfect magnetic crystals is presented which shows that when the magnetization is perpendicular to the diffraction vector (β- π/2), the dispersion surface is made up of two hyperbolic surfaces corresponding to simple polarization states and the results of the two-beam dynamical theory for non-magnetic crystals can be directly applied. The asymptotic properties of the dispersion surface are of the dispersion surface are also discussed in the more general case (β is not equal to π/2) and an analytical treatment of the kinematical limit is presented. Integrated intensities and flipping ratios outside this limit can only be calculated numerically. It is shown that the wave fields defined by the different points of the dispersion surface are polarized in the (g, B 0 ) plane; this is a generalization of the fact that they are (+-) states with respect to B 0 in the simple case (β=π/2). (UK)

  17. Study of Inverse Ni-based Photonic Crystal using the Microradian X-ray Diffraction

    Science.gov (United States)

    Vasilieva, A. V.; Grigoryeva, N. A.; Mistonov, A. A.; Sapoletova, N. A.; Napolskii, K. S.; Eliseev, A. A.; Lukashin, A. V.; Tretyakov, Yu D.; Petukhov, A. V.; Byelov, D.; Chernyshov, D.; Okorokov, A. I.; Bouwman, W. G.; Grigoriev, S. V.

    2010-10-01

    Inverse photonic nickel-based crystal films formed by electrocrystallization of metal inside the voids of polymer artificial opal have been studied using the microradian X-ray diffraction. Analysis of the diffraction images agrees with an face-centred cubic (FCC) structure with the lattice constant a0 = 650 ± 10 nm and indicates two types of stacking sequences coexisting in the crystal (twins of ABCABC... and ACBACB... ordering motifs), the ratio between them being 4:5 The transverse structural correlation length Ltran is 2.4 ± 0.1 μm, which corresponds to a sample thickness of 6 layers. The in-plane structural correlation length Llong is 3.4 ± 0.2 μm, and the structure mosaic is of order of 10°.

  18. Study of Inverse Ni-based Photonic Crystal using the Microradian X-ray Diffraction

    International Nuclear Information System (INIS)

    Vasilieva, A V; Okorokov, A I; Grigoriev, S V; Grigoryeva, N A; Mistonov, A A; Sapoletova, N A; Napolskii, K S; Eliseev, A A; Lukashin, A V; Tretyakov, Yu D; Petukhov, A V; Byelov, D; Chernyshov, D; Bouwman, W G

    2010-01-01

    Inverse photonic nickel-based crystal films formed by electrocrystallization of metal inside the voids of polymer artificial opal have been studied using the microradian X-ray diffraction. Analysis of the diffraction images agrees with an face-centred cubic (FCC) structure with the lattice constant a 0 = 650 ± 10 nm and indicates two types of stacking sequences coexisting in the crystal (twins of ABCABC... and ACBACB... ordering motifs), the ratio between them being 4:5 The transverse structural correlation length L tran is 2.4 ± 0.1 μm, which corresponds to a sample thickness of 6 layers. The in-plane structural correlation length L long is 3.4 ± 0.2 μm, and the structure mosaic is of order of 10 0 .

  19. Study of Inverse Ni-based Photonic Crystal using the Microradian X-ray Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Vasilieva, A V; Okorokov, A I; Grigoriev, S V [Petersburg Nuclear Physics Institute, Gatchina, 188350, St. Petersburg (Russian Federation); Grigoryeva, N A; Mistonov, A A [Department of Physics, St. Petersburg State University, 198504, St. Petersburg (Russian Federation); Sapoletova, N A; Napolskii, K S; Eliseev, A A; Lukashin, A V; Tretyakov, Yu D [Department of Materials Science, Moscow State University, 119899, Moscow (Russian Federation); Petukhov, A V; Byelov, D [Debye Institute, Utrecht University, 3584 CH Utrecht (Netherlands); Chernyshov, D [SNBL European Synchrotron Radiation Facility (ESRF), 38043 Grenoble (France); Bouwman, W G, E-mail: vasilieva@lns.pnpi.spb.r [Delft Technical University, 2629 JB Delft (Netherlands)

    2010-10-01

    Inverse photonic nickel-based crystal films formed by electrocrystallization of metal inside the voids of polymer artificial opal have been studied using the microradian X-ray diffraction. Analysis of the diffraction images agrees with an face-centred cubic (FCC) structure with the lattice constant a{sub 0} = 650 {+-} 10 nm and indicates two types of stacking sequences coexisting in the crystal (twins of ABCABC... and ACBACB... ordering motifs), the ratio between them being 4:5 The transverse structural correlation length L{sub tran} is 2.4 {+-} 0.1 {mu}m, which corresponds to a sample thickness of 6 layers. The in-plane structural correlation length L{sub long} is 3.4 {+-} 0.2 {mu}m, and the structure mosaic is of order of 10{sup 0}.

  20. Synthesis, growth, crystal structure, optical and third order nonlinear optical properties of quinolinium derivative single crystal: PNQI

    Science.gov (United States)

    Karthigha, S.; Krishnamoorthi, C.

    2018-03-01

    An organic quinolinium derivative nonlinear optical (NLO) crystal, 1-ethyl-2-[2-(4-nitro-phenyl)-vinyl]-quinolinium iodide (PNQI) was synthesized and successfully grown by slow evaporation solution growth technique. Formation of a crystalline compound was confirmed by single crystal X-ray diffraction. The quinolinium compound PNQI crystallizes in the triclinic crystal system with a centrosymmetric space group of P-1 symmetry. The molecular structure of PNQI was confirmed by 1H NMR and 13C NMR spectral studies. The thermal properties of the crystal have been investigated by thermogravimetric (TG) and differential scanning calorimetry (DSC) studies. The optical characteristics obtained from UV-Vis-NIR spectral data were described and the cut-off wavelength observed at 506 nm. The etching study was performed to analyse the growth features of PNQI single crystal. The third order NLO properties such as nonlinear refractive index (n2), nonlinear absorption coefficient (β) and nonlinear susceptibility (χ (3)) of the crystal were investigated using Z-scan technique at 632.8 nm of Hesbnd Ne laser.

  1. Press forging of single crystal calcium fluoride

    International Nuclear Information System (INIS)

    Turk, R.R.

    1975-01-01

    Single crystals of high-purity calcium fluoride have been deformed uniaxially in an attempt to improve strength and resistance to cleavage, without impairing infrared transmission. Order of magnitude increases in strength, such as those found in forged KCl, have not been attained, but fine-grained polycrystalling material has been produced which is resistant to crystalline cleavage. Deformation rates of 10 -2 min -1 , reductions of 10 to 73 percent in height, and deformation temperatures of 550 to 1000 0 C have been used. Flexural strengths over 13,000 psi and grain sizes down to 5 μm have been obtained. Reduction of residual stress through heat treatment has been studied, and resultant techniques applied before, during, and after deformation. No increase in infrared absorption has been noted at the CO laser wavelength of 5.3 μm

  2. Electronic structure of single crystal C60

    International Nuclear Information System (INIS)

    Wu, J.; Shen, Z.X.; Dessau, D.S.; Cao, R.; Marshall, D.S.; Pianetta, P.; Lindau, I.; Yang, X.; Terry, J.; King, D.M.; Wells, B.O.; Elloway, D.; Wendt, H.R.; Brown, C.A.; Hunziker, H.; Vries, M.S. de

    1992-01-01

    We report angle-resolved photoemission data from single crystals of C 60 cleaved in UHV. Unlike the other forms of pure carbon, the valence band spectrum of C 60 consists of many sharp features that can be essentially accounted for by the quantum chemical calculations describing individual molecules. This suggests that the electronic structure of solid C 60 is mainly determined by the bonding interactions within the individual molecules. We also observe remarkable intensity modulations of the photoemission features as a function of photon energy, suggesting strong final state effects. Finally, we address the issue of the band width of the HOMO state of C 60 . We assert that the width of the photoemission peak of C 60 does not reflect the intrinsic band width because it is broadened by the non 0-0 transitions via the Franck-Condon principle. Our view point provides a possible reconciliation between these photoemission data and those measured by other techniques. (orig.)

  3. Photoluminescent properties of single crystal diamond microneedles

    Science.gov (United States)

    Malykhin, Sergey A.; Ismagilov, Rinat R.; Tuyakova, Feruza T.; Obraztsova, Ekaterina A.; Fedotov, Pavel V.; Ermakova, Anna; Siyushev, Petr; Katamadze, Konstantin G.; Jelezko, Fedor; Rakovich, Yury P.; Obraztsov, Alexander N.

    2018-01-01

    Single crystal needle-like diamonds shaped as rectangular pyramids were produced by combination of chemical vapor deposition and selective oxidation with dimensions and geometrical characteristics depending on the deposition process parameters. Photoluminescence spectra and their dependencies on wavelength of excitation radiation reveal presence of nitrogen- and silicon-vacancy color centers in the diamond crystallites. Photoluminescence spectra, intensity mapping, and fluorescence lifetime imaging microscopy indicate that silicon-vacancy centers are concentrated at the crystallites apex while nitrogen-vacancy centers are distributed over the whole crystallite. Dependence of the photoluminescence on excitation radiation intensity demonstrates saturation and allows estimation of the color centers density. The combination of structural parameters, geometry and photoluminescent characteristics are prospective for advantageous applications of these diamond crystallites in quantum information processing and optical sensing.

  4. Hydrogen Annealing Of Single-Crystal Superalloys

    Science.gov (United States)

    Smialek, James L.; Schaeffer, John C.; Murphy, Wendy

    1995-01-01

    Annealing at temperature equal to or greater than 2,200 degrees F in atmosphere of hydrogen found to increase ability of single-crystal superalloys to resist oxidation when subsequently exposed to oxidizing atmospheres at temperatures almost as high. Supperalloys in question are principal constituents of hot-stage airfoils (blades) in aircraft and ground-based turbine engines; also used in other high-temperature applications like chemical-processing plants, coal-gasification plants, petrochemical refineries, and boilers. Hydrogen anneal provides resistance to oxidation without decreasing fatigue strength and without need for coating or reactive sulfur-gettering constituents. In comparison with coating, hydrogen annealing costs less. Benefits extend to stainless steels, nickel/chromium, and nickel-base alloys, subject to same scale-adhesion and oxidation-resistance considerations, except that scale is chromia instead of alumina.

  5. EPR of CU+2:Mb single crystal

    International Nuclear Information System (INIS)

    Nascimento, O.R.; Ribeiro, S.C.; Bemski, G.

    1976-01-01

    Copper introduced into met-myoglobin crystals occupies various sites as indicated by EPR parameters. CU 2+ (A) is probably liganded to histidine A10, lysine A14 and asparagine GH4 (Banaszak, 1965) and shows super-hyperfine interaction with a single (imidazole) nitrogen. Cu 2+ (B) and Cu 2+ (C) correspond to other anisotropic sites described with lesser details. Cu 2+ (A) exhibits a transition to an isotropic form with a transition temperature of 40.5 0 C. This transition is indicative of a conformational change in myoglobin and could correspond to a motion of A helix away from the GH section. The transition temperature is 7 0 C higher than the previously reported (Atanasov, 1971) one for myoglobin in solution

  6. New structural studies of liquid crystal by reflectivity and resonant X-ray diffraction; Nouvelles etudes structurales de cristaux liquides par reflectivite et diffraction resonante des rayons X

    Energy Technology Data Exchange (ETDEWEB)

    Fernandes, P

    2007-04-15

    This memory presents three structural studies of smectic Liquid Crystals by reflectivity and resonant diffraction of X-rays. It is divided in five chapters. In the first a short introduction to Liquid Crystals is given. In particular, the smectic phases that are the object of this study are presented. The second chapter is consecrated to the X-ray experimental techniques that were used in this work. The three last chapters present the works on which this thesis can be divided. Chapter three demonstrates on free-standing films of MHPOBC (historic liquid crystal that possesses the antiferroelectric sub-phases) the possibility to extend the technique of resonant X-ray diffraction to liquid crystals without resonant element. In the fourth chapter the structure of the B{sub 2} liquid crystal phase of bent-core molecules (or banana molecules) is elucidated by using resonant X-ray diffraction combined with polarization analysis of the diffracted beam. A model of the polarization of the resonant beam diffracted by four different structures proposed for the B{sub 2} phase is developed in this chapter. In the fifth chapter a smectic binary mixture presenting a very original critical point of phase separation is studied by X-ray reflectivity and optical microscopy. A concentration gradient in the direction perpendicular to the plane of the film seems to be induced by the free-standing film geometry. The results of a simplified model of the system are compatible with this interpretation.

  7. Chlorination of irradiated polyethylene single crystals

    International Nuclear Information System (INIS)

    Grimm, H.J.

    1978-01-01

    The chlorination of electron beam-irradiation polyethylene (PE) single crystals was studied for a range of irradiation doses, temperatures, and chlorine interaction times. The results presented show that PE chlorination was quite extensive, even in unirradiated PE single crystals at 25 0 C in the dark. Electron Spin Resonance (ESR, EPR) was used in this study in order to determine the alkyl radical concentration, decay constant, and diffusivity for (unchlorinated) specimens. An alkyl radical diffusivity D/sub a/ = 1.6 x 10 -17 cm 2 /sec at 25 0 C was estimated from ESR data and alkyl radical migration as one-dimensional unsteady-state diffusion process. In irradiated PE, chlorination occurred mainly via chain reactions which were initiated by the irradiation-produced free radicals. Chlorine content values were determined by X-ray Energy Spectroscopy (XES). It was found that the magnitude of the chlorine uptake increased with increasing dose, and decreased with decreasing temperature at constant dose. Otherwise the observed PE chlorination phenomena was quite similar for all of the doses and temperatures studied here, consisting of a two step mechanism: a fast uptake which occurred between time tCl 2 = 0 - 5 minutes and a slower, approximately first-order rate of uptake which occurred between times tCl 2 = 5 - 120 minutes. Chlorination was essentially complete by time tCl 2 = 120 minutes. The rapid uptake probably occurred in the amorphous surface zones where Cl 2 is relatively high and the second, slower step was probably attributable to Cl 2 diffusion into the crystalline regions and subsequent chlorination there. Inasmuch as the PE density decreases with increasing dose (for 1-600 Mrad), Cl 2 diffusivity was enhanced, resulting in higher chlorine uptake values at higher doses

  8. Validation of a Crystal Plasticity Model Using High Energy Diffraction Microscopy

    Science.gov (United States)

    Beaudoin, A. J.; Obstalecki, M.; Storer, R.; Tayon, W.; Mach, J.; Kenesei, P.; Lienert, U.

    2012-01-01

    High energy diffraction microscopy is used to measure the crystallographic orientation and evolution of lattice strain in an Al Li alloy. The relative spatial arrangement of the several pancake-shaped grains in a tensile sample is determined through in situ and ex situ techniques. A model for crystal plasticity with continuity of lattice spin is posed, where grains are represented by layers in a finite element mesh following the arrangement indicated by experiment. Comparison is drawn between experiment and simulation.

  9. Expression, purification, crystallization and preliminary X-ray diffraction analysis of nurse shark β2-microglobulin

    OpenAIRE

    Lu, Shuangshuang; Yao, Shugang; Chen, Rong; Zhang, Nianzhi; Chen, Jianmin; Gao, Feng; Xia, Chun

    2012-01-01

    A crystal of nurse shark β2-microglobulin diffracted to 2.3 Å resolution and belonged to space group P3221, with unit-cell parameters a = b = 88.230, c = 67.146 Å and two molecules per asymmetric unit. The Matthews coefficient V M was calculated to be about 3.28 Å3 Da−1, corresponding to 62.5% solvent content.

  10. Time and space domain separation of pulsed X-ray beams diffracted from vibrating crystals

    Energy Technology Data Exchange (ETDEWEB)

    Nosik, V. L., E-mail: v-nosik@yandex.ru, E-mail: nosik@ns.crys.ras.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics,” (Russian Federation)

    2016-11-15

    It is known that a set of additional reflections (satellites) may arise on rocking curves in the case of X-ray diffraction in the Bragg geometry from crystals where high-frequency ultrasonic vibrations are excited. It is shown that, under certain conditions, the pulse wave fields of the satellites and main reflection may be intersected in space (playing the role of pump and probe beams) and in time (forming interference superlattices).

  11. Moessbauer diffraction study of the Neel phase transition in Fe3BO6 crystal

    International Nuclear Information System (INIS)

    Kovalenko, P.P.; Labushkin, V.G.; Sarkisov, Eh.R.; Tolpekin, I.G.

    1987-01-01

    Phase transitions in a 57 Fe 3 BO 6 monocrystal in the vicinity of the Neel point, T N =507.5 K were investigated by means of the Moessbauergraphy. For the first time the relaxation type of Moessbauer spectra was observed near the phase transition point. First in the Moessbauer diffraction spectrum of the crystal the simultaneous presence of a component resulted from magnetic ordering and a paramagnetic component was observed

  12. Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation

    Czech Academy of Sciences Publication Activity Database

    Hrdý, Jaromír; Mikulík, P.; Oberta, Peter

    2011-01-01

    Roč. 18, č. 2 (2011), s. 299-301 ISSN 0909-0495 R&D Projects: GA MPO FR-TI1/412 Institutional research plan: CEZ:AV0Z10100522 Keywords : diffractive-refractive optics * x-ray synchrotron radiation monochromator * x-ray crystal monochromator * harmonics separation Subject RIV: BH - Optics, Masers, Lasers Impact factor: 2.726, year: 2011

  13. Neutron diffraction study of single crystalline ErCo10Mo2

    International Nuclear Information System (INIS)

    Janssen, Y.; De Boer, F.R.; Brueck, E.; Tegus, O.; Ma, L.; Buschow, K.H.J.; Reehuis, M.

    1999-01-01

    Complete text of publication follows. The ferrimagnetic intermetallic compound ErCo 10 Mo 2 (Tc = 600 K) crystallizes in the tetragonal ThMn 12 -type structure (space group 14/mmm). The Co and Mo atoms may share three crystallographic sites (8f, 8i and 8j). Earlier neutron powder diffraction experiments show that Mo has a strong preference for the 8i-site and that the magnetic ordering at low temperature is planar. Furthermore ErCo 10 Mo 2 has been reported to show one [2] or more [3] spin-reorientation transitions from planar to axial magnetic ordering. Recently we succeeded in growing a single-crystalline sample of ErCo 10 Mo 2 . Magnetic measurements in 1T show one spin-reorientation transition at about 135 K. Neutron diffraction experiments were performed to investigate a possible link between the magnetic properties and the site occupation by Mo. Our results show that our sample has the Mo atoms exclusively occupying half the 8i-sites. There is no evidence for a crystallographic superstructure. Furthermore, below 150 K some reflections strongly increase due to the growing Er magnetic moment. (author)

  14. Neutron beam applications - Development of single crystal structure analysis technique using the HANARO neutron four circle diffractometer

    Energy Technology Data Exchange (ETDEWEB)

    Suh, Il Hwan; Kim, Moon Jib; Kim, Jin Gyu [Chungnam National University, Taejon (Korea)

    2000-04-01

    As the four circle diffractometer (FCD) has been set up in HANARO, it has become possible to study the single crystal structures by means of the neutron diffraction. Taking account of the geometry of the FCD, a program for the control of te FCD and neutron data acquisition operating under Windows' circumstance has been accomplished. Also, a computer program which can automatically measure the diffraction intensity data has been developed. All data obtained from the FCD are processed automatically for further work and a software for the single crystal structure analyses has been prepared. A KC1 single crystal was selected as first test sample for a structure analysis had been successfully performed on the FCD using in-house developed program and accordingly their functionings with precision were confirmed. For regular single crystal diffraction experiments, the structure analyses of chrysoberyl and Zr(Y)0{sub 1.87} single crystals were performed using both neutron and X-ray diffraction methods, and the result showed that the neutron diffraction work is superior to the X-ray one from the viewpoint of certain crystallographic information obtainable only from the former one. 24 refs., 15 figs., 15 tabs. (Author)

  15. Crystallization and preliminary X-ray diffraction analysis of diaminopimelate epimerase from Escherichia coli

    International Nuclear Information System (INIS)

    Hor, Lilian; Dobson, Renwick C. J.; Dogovski, Con; Hutton, Craig A.; Perugini, Matthew A.

    2009-01-01

    Diaminopimelate (DAP) epimerase, an enzyme in the lysine-biosynthetic pathway, is a promising target for antibiotic development against pathogenic bacteria. Here, the cloning, expression, purification, crystallization and preliminary diffraction analysis of DAP epimerase from E. coli are reported. Diaminopimelate (DAP) epimerase (EC 5.1.1.7) catalyzes the penultimate step of lysine biosynthesis in bacteria and plants, converting l,l-diaminopimelate to meso-diaminopimelate. Here, the cloning, expression, purification, crystallization and preliminary X-ray diffraction analysis of DAP epimerase from Escherichia coli are presented. Crystals were obtained in space group P4 1 2 1 2 and diffracted to 2.0 Å resolution, with unit-cell parameters a = b = 89.4, c = 179.6 Å. Molecular replacement was conducted using Bacillus anthracis DAP epimerase as a search model and showed the presence of two molecules in the asymmetric unit, with an initial R free of 0.456 and R work of 0.416

  16. Single-crystal growth of ceria-based materials; Einkristallzuechtung von Materialien auf der Basis von Cerdioxid

    Energy Technology Data Exchange (ETDEWEB)

    Ulbrich, Gregor

    2015-07-23

    In this work it could be shown that Skull-Melting is a suitable method for growing ceria single crystals. Twenty different ceria-based single crystals could be manufactured. It was possible to dope ceria single crystals with Gd, Sm, Y, Zr, Ti, Ta, and Pr in different concentrations. Also co-doping with the named metals was realized. However, there remain some problems for growing ceria-based single crystals by Skull-Melting. As ignition metal zirconium was used because no ceria-based material works well. For that reason all single crystals show small zirconium contamination. Another problem is the formation of oxygen by the heat-induced reduction of ceria during the melting process. Because of that the skull of sintered material is often destroyed by gas pressure. This problem had to be solved individually for every single crystal. The obtained single crystals were characterized using different methods. To ensure the single crystal character the y were examined by Laue diffraction. All manufactured crystals are single crystals. Also powder diffraction patterns of the milled and oxidized samples were measured. For the determination of symmetry and metric the structural parameters were analyzed by the Rietveld method. All synthesized materials crystallize in space group Fm-3m known from calcium fluoride. The cubic lattice parameter a was determined for all crystals. In the case of series with different cerium and zirconium concentrations a linear correlation between cerium content and cubic lattice parameter was detected. The elemental composition was determined by WDX. All crystals show a homogeneous elemental distribution. The oxygen content was calculated because the WDX method isn't useful for determination.

  17. Perdeuteration, purification, crystallization and preliminary neutron diffraction of an ocean pout type III antifreeze protein

    International Nuclear Information System (INIS)

    Petit-Haertlein, Isabelle; Blakeley, Matthew P.; Howard, Eduardo; Hazemann, Isabelle; Mitschler, Andre; Haertlein, Michael; Podjarny, Alberto

    2009-01-01

    Perdeuterated type III antifreeze protein has been expressed, purified and crystallized. Preliminary neutron data collection showed diffraction to 1.85 Å resolution from a 0.13 mm 3 crystal. The highly homologous type III antifreeze protein (AFP) subfamily share the capability to inhibit ice growth at subzero temperatures. Extensive studies by X-ray crystallography have been conducted, mostly on AFPs from polar fishes. Although interactions between a defined flat ice-binding surface and a particular lattice plane of an ice crystal have now been identified, the fine structural features underlying the antifreeze mechanism still remain unclear owing to the intrinsic difficulty in identifying H atoms using X-ray diffraction data alone. Here, successful perdeuteration (i.e. complete deuteration) for neutron crystallographic studies of the North Atlantic ocean pout (Macrozoarces americanus) AFP in Escherichia coli high-density cell cultures is reported. The perdeuterated protein (AFP D) was expressed in inclusion bodies, refolded in deuterated buffer and purified by cation-exchange chromatography. Well shaped perdeuterated AFP D crystals have been grown in D 2 O by the sitting-drop method. Preliminary neutron Laue diffraction at 293 K using LADI-III at ILL showed that with a few exposures of 24 h a very low background and clear small spots up to a resolution of 1.85 Å were obtained using a ‘radically small’ perdeuterated AFP D crystal of dimensions 0.70 × 0.55 × 0.35 mm, corresponding to a volume of 0.13 mm 3

  18. Optical properties of tungsten disulfide single crystals doped with gold

    International Nuclear Information System (INIS)

    Dumcenco, D.O.; Hsu, H.P.; Huang, Y.S.; Liang, C.H.; Tiong, K.K.; Du, C.H.

    2008-01-01

    Single crystals of WS 2 doped with gold have been grown by the chemical vapour transport method using iodine as a transporting agent. X-ray diffraction (XRD) pattern analysis revealed presence of mixed three-layer rhombohedral (3R) and two-layer hexagonal (2H) polytypes for the doped crystals while the undoped one shows only 2H form. Hall measurements indicate that the samples are p-type in nature. The doping effects of the materials are characterized by surface photovoltage (SPV), photoconductivity (PC) and piezoreflectance (PzR) measurements. Room temperature SPV and PC spectra reveal a feature located at ∼60 meV below the A exciton and has been tentatively assigned to be an impurity level caused by Au dopant. Excitonic transition energies of the A, B, d and C excitons detected in PzR spectra show red shift due to the presence of a small amount of Au and the broadening parameters of the excitonic transition features increase due to impurity scattering. The values of the parameters that describe the electron (exciton)-phonon interaction of excitonic transitions of A-B are about two times larger than that of d-C excitonic pairs. The possible assignments of the different origins of A-B and d-C excitonic pairs have been discussed

  19. Crystallization and X-ray diffraction analysis of the Trp/amber editing site of hepatitis delta virus (+)RNA: a case of rational design

    International Nuclear Information System (INIS)

    MacElrevey, Celeste; Wedekind, Joseph E.

    2005-01-01

    Well diffracting decamer crystals of the hepatitis delta virus RNA-editing site were prepared, but exhibited merohedral twinning and base averaging owing to duplex symmetry. A longer asymmetric construct that includes additional flanking RNA sequences has been crystallized that does not appear to exhibit these defects. RNA editing by mammalian ADAR1 (Adenosine Deaminase Acting on RNA) is required for the life cycle of the hepatitis delta virus (HDV). Editing extends the single viral open reading frame to yield two protein products of alternate length. ADARs are believed to recognize double-stranded RNA substrates via a ‘structure-based’ readout mechanism. Crystals of 10-mer duplexes representing the HDV RNA-editing site diffracted to 1.35 Å resolution, but suffered from merohedral twinning and averaging of the base registry. Expansion of the construct to include two flanking 3 × 1 internal loops yielded crystals in the primitive tetragonal space group P4 1 2 1 2 or P4 3 2 1 2. X-ray diffraction data were collected to 2.8 Å resolution, revealing a unit cell with parameters a = 62.5, c = 63.5 Å. The crystallization and X-ray analysis of multiple forms of the HDV RNA-editing substrate, encounters with common RNA crystal-growth defects and a strategy to overcome these problems are reported

  20. Orientation dependence of the thermal fatigue of nickel alloy single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Dul' nev, R A; Svetlov, I L; Bychkov, N G; Rybina, T V; Sukhanov, N N

    1988-11-01

    The orientation dependence of the thermal stability and the thermal fatigue fracture characteristics of single crystals of MAR-M200 nickel alloy are investigated experimentally using X-ray diffraction analysis and optical and scanning electron microscopy. It is found that specimens with the 111-line orientation have the highest thermal stability and fatigue strength. Under similar test conditions, the thermal fatigue life of single crystals is shown to be a factor of 1.5-2 higher than that of the directionally solidified and equiaxed alloys. 6 references.

  1. Crystallization and preliminary diffraction studies of SFC-1, a carbapenemase conferring antibiotic resistance

    International Nuclear Information System (INIS)

    Hong, Myoung-Ki; Lee, Jae Jin; Wu, Xing; Kim, Jin-Kwang; Jeong, Byeong Chul; Pham, Tan-Viet; Kim, Seung-Hwan; Lee, Sang Hee; Kang, Lin-Woo

    2012-01-01

    The SFC-1 gene from S. fonticola was cloned and SFC-1 was expressed, purified and crystallized. X-ray diffraction data were collected from an SFC-1 crystal to 1.6 Å resolution. SFC-1, a class A carbapenemase that confers antibiotic resistance, hydrolyzes the β-lactam rings of β-lactam antibiotics (carbapenems, cephalosporins, penicillins and aztreonam). SFC-1 presents an enormous challenge to infection control, particularly in the eradication of Gram-negative pathogens. As SFC-1 exhibits a remarkably broad substrate range, including β-lactams of all classes, the enzyme is a potential target for the development of antimicrobial agents against pathogens producing carbapenemases. In this study, SFC-1 was cloned, overexpressed, purified and crystallized. The SFC-1 crystal diffracted to 1.6 Å resolution and belonged to the orthorhombic space group P2 1 2 1 2 1 , with unit-cell parameters a = 65.8, b = 68.3, c = 88.8 Å. Two molecules are present in the asymmetric unit, with a corresponding V M of 1.99 Å 3 Da −1 and a solvent content of 38.1%

  2. Expression, purification, crystallization and preliminary X-ray diffraction analysis of nurse shark β2-microglobulin

    International Nuclear Information System (INIS)

    Lu, Shuangshuang; Yao, Shugang; Chen, Rong; Zhang, Nianzhi; Chen, Jianmin; Gao, Feng; Xia, Chun

    2012-01-01

    A crystal of nurse shark β 2 -microglobulin diffracted to 2.3 Å resolution and belonged to space group P3 2 21, with unit-cell parameters a = b = 88.230, c = 67.146 Å and two molecules per asymmetric unit. The Matthews coefficient V M was calculated to be about 3.28 Å 3 Da −1 , corresponding to 62.5% solvent content. β 2 -Microglobulin (β 2 m) is an essential subunit of the major histocompatibility complex (MHC) class I molecule that helps to stabilize the structure of peptide–MHC I (pMHC I). It is also one of the typical immunoglobulin superfamily (IgSF) molecules in the adaptive immune system (AIS). Sharks belong to the cartilaginous fish, which are the oldest jawed vertebrate ancestors with an AIS to exist in the world. Thus, the study of cartilaginous fish β 2 m would help in understanding the evolution of IgSF molecules. In order to demonstrate this, β 2 m from a cartilaginous fish, nurse shark (Ginglymostoma cirratum), was expressed, refolded, purified and crystallized. Diffraction data were collected to a resolution of 2.3 Å. The crystal belonged to space group P3 2 21, with unit-cell parameters a = b = 88.230, c = 67.146 Å. The crystal structure contained two molecules in the asymmetric unit. The results will provide structural information for study of the evolution of β 2 m and IgSF in the AIS

  3. Crystallization and preliminary X-ray diffraction analysis of Nsp15 from SARS coronavirus

    International Nuclear Information System (INIS)

    Ricagno, Stéfano; Coutard, Bruno; Grisel, Sacha; Brémond, Nicolas; Dalle, Karen; Tocque, Fabienne; Campanacci, Valérie; Lichière, Julie; Lantez, Violaine; Debarnot, Claire; Cambillau, Christian; Canard, Bruno; Egloff, Marie-Pierre

    2006-01-01

    Crystals of Nsp15 from the aetiological agent of SARS have been grown at room temperature. Crystals have cubic symmetry and diffract to a maximum resolution of 2.7 Å. The non-structural protein Nsp15 from the aetiological agent of SARS (severe acute respiratory syndrome) has recently been characterized as a uridine-specific endoribonuclease. This enzyme plays an essential role in viral replication and transcription since a mutation in the related H229E human coronavirus nsp15 gene can abolish viral RNA synthesis. SARS full-length Nsp15 (346 amino acids) has been cloned and expressed in Escherichia coli with an N-terminal hexahistidine tag and has been purified to homogeneity. The protein was subsequently crystallized using PEG 8000 or 10 000 as precipitants. Small cubic crystals of the apoenzyme were obtained from 100 nl nanodrops. They belong to space group P4 1 32 or P4 3 32, with unit-cell parameters a = b = c = 166.8 Å. Diffraction data were collected to a maximum resolution of 2.7 Å

  4. Crystallization and preliminary X-ray diffraction analysis of human endoplasmic reticulum aminopeptidase 2

    International Nuclear Information System (INIS)

    Ascher, David B.; Polekhina, Galina; Parker, Michael W.

    2012-01-01

    The luminal domain of human endoplasmic reticulum aminopeptidase 2 has been expressed, purified and crystallized. The crystals belonged to the orthorhombic space group P2 1 2 1 2 and diffracted anisotropically to 3.3 Å resolution in the best direction on an in-house source. Endoplasmic reticulum aminopeptidase 2 (ERAP2) is a critical enzyme involved in the final processing of MHC class I antigens. Peptide trimming by ERAP2 and the other members of the oxytocinase subfamily is essential to customize longer precursor peptides in order to fit them to the correct length required for presentation on major histocompatibility complex class I molecules. While recent structures of ERAP1 have provided an understanding of the ‘molecular-ruler’ mechanism of substrate selection, little is known about the complementary activities of its homologue ERAP2 despite their sharing 49% sequence identity. In order to gain insights into the structure–function relationship of the oxytocinase subfamily, and in particular ERAP2, the luminal region of human ERAP2 has been crystallized in the presence of the inhibitor bestatin. The crystals belonged to an orthorhombic space group and diffracted anisotropically to 3.3 Å resolution in the best direction on an in-house X-ray source. A molecular-replacement solution suggested that the enzyme has adopted the closed state as has been observed in other inhibitor-bound aminopeptidase structures

  5. Crystallization and preliminary X-ray diffraction analysis of Nsp15 from SARS coronavirus

    Energy Technology Data Exchange (ETDEWEB)

    Ricagno, Stéfano; Coutard, Bruno; Grisel, Sacha; Brémond, Nicolas; Dalle, Karen; Tocque, Fabienne; Campanacci, Valérie; Lichière, Julie; Lantez, Violaine; Debarnot, Claire; Cambillau, Christian; Canard, Bruno; Egloff, Marie-Pierre, E-mail: marie-pierre.egloff@afmb.univ-mrs.fr [Centre National de la Recherche Scientifique and Universités d’Aix-Marseille I et II, UMR 6098, Architecture et Fonction des Macromolécules Biologiques, Ecole Supérieure d’Ingénieurs de Luminy-Case 925, 163 Avenue de Luminy, 13288 Marseille CEDEX 9 (France)

    2006-04-01

    Crystals of Nsp15 from the aetiological agent of SARS have been grown at room temperature. Crystals have cubic symmetry and diffract to a maximum resolution of 2.7 Å. The non-structural protein Nsp15 from the aetiological agent of SARS (severe acute respiratory syndrome) has recently been characterized as a uridine-specific endoribonuclease. This enzyme plays an essential role in viral replication and transcription since a mutation in the related H229E human coronavirus nsp15 gene can abolish viral RNA synthesis. SARS full-length Nsp15 (346 amino acids) has been cloned and expressed in Escherichia coli with an N-terminal hexahistidine tag and has been purified to homogeneity. The protein was subsequently crystallized using PEG 8000 or 10 000 as precipitants. Small cubic crystals of the apoenzyme were obtained from 100 nl nanodrops. They belong to space group P4{sub 1}32 or P4{sub 3}32, with unit-cell parameters a = b = c = 166.8 Å. Diffraction data were collected to a maximum resolution of 2.7 Å.

  6. Preliminary neutron diffraction analysis of challenging human manganese superoxide dismutase crystals.

    Science.gov (United States)

    Azadmanesh, Jahaun; Trickel, Scott R; Weiss, Kevin L; Coates, Leighton; Borgstahl, Gloria E O

    2017-04-01

    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, methods are presented for large crystal growth and neutron data collection of human manganese SOD (MnSOD) using perdeuteration and the MaNDi beamline at Oak Ridge National Laboratory. 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 been collected via neutron diffraction to sufficient resolution (2.30 Å) where hydrogen positions can be observed.

  7. Purification, crystallization and preliminary X-ray diffraction analysis of the glyoxalase II from Leishmania infantum

    International Nuclear Information System (INIS)

    Trincão, José; Sousa Silva, Marta; Barata, Lídia; Bonifácio, Cecília; Carvalho, Sandra; Tomás, Ana Maria; Ferreira, António E. N.; Cordeiro, Carlos; Ponces Freire, Ana; Romão, Maria João

    2006-01-01

    A glyoxalase II from L. infantum was cloned, purified and crystallized and its structure was solved by X-ray crystallography. In trypanosomatids, trypanothione replaces glutathione in all glutathione-dependent processes. Of the two enzymes involved in the glyoxalase pathway, glyoxalase I and glyoxalase II, the latter shows absolute specificity towards trypanothione thioester, making this enzyme an excellent model to understand the molecular basis of trypanothione binding. Cloned glyoxalase II from Leishmania infantum was overexpressed in Escherichia coli, purified and crystallized. Crystals belong to space group C222 1 (unit-cell parameters a = 65.6, b = 88.3, c = 85.2 Å) and diffract beyond 2.15 Å using synchrotron radiation. The structure was solved by molecular replacement using the human glyoxalase II structure as a search model. These results, together with future detailed kinetic characterization using lactoyltrypanothione, should shed light on the evolutionary selection of trypanothione instead of glutathione by trypano-somatids

  8. Hard X-ray diffraction enhanced imaging only using two crystals

    Institute of Scientific and Technical Information of China (English)

    LI Gang; WANG Nan; WU Ziyu

    2004-01-01

    Different configurations for the monochromator crystals and the analyzer crystals have been used in hard X-ray diffraction enhanced imaging (DEI) methods to overcome the complex task to adjust each of them to the ideal position. Here we present a very compact DEI configuration, and preliminary results of experiments performed at the Beijing Synchrotron Radiation Facility (BSRF) using only two crystals: the first one acting as monochromator and the second one as analyzer in the Bragg geometry. Refraction contrast images characterized by high contrast and spatial resolution are obtained and compared with absorption images. Differences among these images will be outlined and discussed emphasizing the potential capabilities of this very simple layout that guarantees a high transmission efficiency.

  9. Validation of molecular crystal structures from powder diffraction data with dispersion-corrected density functional theory (DFT-D).

    Science.gov (United States)

    van de Streek, Jacco; Neumann, Marcus A

    2014-12-01

    In 2010 we energy-minimized 225 high-quality single-crystal (SX) structures with dispersion-corrected density functional theory (DFT-D) to establish a quantitative benchmark. For the current paper, 215 organic crystal structures determined from X-ray powder diffraction (XRPD) data and published in an IUCr journal were energy-minimized with DFT-D and compared to the SX benchmark. The on average slightly less accurate atomic coordinates of XRPD structures do lead to systematically higher root mean square Cartesian displacement (RMSCD) values upon energy minimization than for SX structures, but the RMSCD value is still a good indicator for the detection of structures that deserve a closer look. The upper RMSCD limit for a correct structure must be increased from 0.25 Å for SX structures to 0.35 Å for XRPD structures; the grey area must be extended from 0.30 to 0.40 Å. Based on the energy minimizations, three structures are re-refined to give more precise atomic coordinates. For six structures our calculations provide the missing positions for the H atoms, for five structures they provide corrected positions for some H atoms. Seven crystal structures showed a minor error for a non-H atom. For five structures the energy minimizations suggest a higher space-group symmetry. For the 225 SX structures, the only deviations observed upon energy minimization were three minor H-atom related issues. Preferred orientation is the most important cause of problems. A preferred-orientation correction is the only correction where the experimental data are modified to fit the model. We conclude that molecular crystal structures determined from powder diffraction data that are published in IUCr journals are of high quality, with less than 4% containing an error in a non-H atom.

  10. Analyses of significant features of L-Prolinium Picrate single crystal: An excellent material for non linear optical applications

    Energy Technology Data Exchange (ETDEWEB)

    Thukral, Kanika [Academy of Scientific and Innovative Research, CSIR- National Physical Laboratory, New Delhi, 110012 (India); CSIR-National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi, 110 012 (India); Vijayan, N., E-mail: nvijayan@nplindia.org [CSIR-National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi, 110 012 (India); Vij, Mahak [CSIR-National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi, 110 012 (India); Nagaraja, C.M. [Department of Chemistry, Indian Institute of Technology Ropar, Rupnagar, 140001, Punjab (India); Jayaramakrishnan, V. [Centro De Investigations En Optica, Loma del Bosque 115, Colonia Lomas del Campestre, León, Guanajuato, Código Postal, 37150 (Mexico); Jayalakshmy, M.S. [International and Inter University Centre for Nanoscience and Nanotechnology, Mahatma Gandhi University, Kottayam, Kerala, 686560 (India); Kant, Rajni [Department of Physics and Electronics, University of Jammu, Jammu Tawi, 180006 (India)

    2017-06-15

    Today the fundamental aspect of the researchers is to explore maximum physical properties of the material for device fabrication. In the present article, single crystal X-ray diffraction has been carried out to verify the formation of the synthesized compound. In addition to that, powder X-ray diffraction has been performed to obtain diffraction pattern of L-Prolinium Picrate single crystal. The strain present inside the single crystal was measured using Hall-Williamson equation from PXRD measurements. The dark current and photon current was obtained from photoconductivity technique whose plot depicted that the sample was negative photoconducting material. Optical homogeneity of the single crystal was analyzed using birefringence technique. Its resistance towards Nd: YAG laser was scrutinized for L-Prolinium Picrate single crystal by applying 1 pulse per second. Different thermal parameters like thermal conductivity, thermal diffusivity, thermal effusivity and specific heat were computed using photo-pyroelectric technique. Solid state parameters were calculated from Clausius Mossotti relation by taking structural information of the title compound. Also, optical parameters like refractive index, reflectance etc were calculated through UV–Vis–NIR analysis. - Highlights: • An optically transparent L-Prolinium Picrate single crystal was harvested from slow evaporation solution growth technique. • The compound shows negative photoconducting nature. • Its optical homogeneity was analyzed using birefringence. • Single shot of laser was applied to sample to measure laser damage threshold value. • The thermal parameters were computed from Photopyroelectric technique.

  11. Influence of the crystal-surface unevenness on the angular spread of an x-ray diffracted beam

    International Nuclear Information System (INIS)

    Hrda, JaromIra; Potlovskiy, Kirill; Hrdy, JaromIr; Slechtova, Venceslava

    2005-01-01

    One of the factors influencing the focus size in diffractive-refractive optics is the quality of diffracting surface. If the surface is uneven, as it is when the silicon crystal surface is only etched, then the diffraction at each point of the surface is a combination of an asymmetric and inclined diffraction (general asymmetric diffraction). This somewhat deviates and spreads the diffracted beam. The integration over the surface hit by an incident beam gives the angular spread of the diffracted beam. It is shown theoretically that in some cases (highly asymmetric, highly inclined cut) the etched surface may create the spread of the diffracted beam such that it causes a significant broadening of the focus. In this case a mechanical-chemical polishing is necessary. This has been verified by us earlier in a preliminary experiment with synchrotron radiation. In this work the new experiment with the same crystals is performed using double crystal (+, -) arrangement and a laboratory x-ray source (CuKα radiation). We compared two samples; one of them is mechanically-chemically (MC) polished and thus the diffracting surface is almost perfect; the other is only etched. This experiment allows a better comparison of the result with the theory. The difference between the measured rocking curve widths for the etched and MC polished crystals (10'') roughly agrees with theory (7''), which supports the correctness of the theoretical approach

  12. Diffracted X-ray tracking: new system for single molecular detection with X-rays

    CERN Document Server

    Sasaki, Y C; Adachi, S; Suzuki, Y; Yagi, N

    2001-01-01

    We propose a new X-ray methodology for direct observations of the behaviors of single molecular units in real time and real space. This new system, which we call Diffracted X-ray Tracking (DXT), monitors the Brownian motions of a single molecular unit by observations of X-ray diffracted spots from a nanocrystal, tightly bound to the individual single molecular unit in bio-systems. DXT does not determine any translational movements, but only orientational movements.

  13. Diffracted X-ray tracking: new system for single molecular detection with X-rays

    International Nuclear Information System (INIS)

    Sasaki, Y.C.; Okumura, Y.; Adachi, S.; Suzuki, Y.; Yagi, N.

    2001-01-01

    We propose a new X-ray methodology for direct observations of the behaviors of single molecular units in real time and real space. This new system, which we call Diffracted X-ray Tracking (DXT), monitors the Brownian motions of a single molecular unit by observations of X-ray diffracted spots from a nanocrystal, tightly bound to the individual single molecular unit in bio-systems. DXT does not determine any translational movements, but only orientational movements

  14. Growth and characterization of Sm3+ doped cerium oxalate single crystals

    Directory of Open Access Journals (Sweden)

    Minu Mary C

    2016-07-01

    Full Text Available Single crystals of Sm3+ doped cerium oxalate decahydrate were synthesized using single diffusion gel technique and the conditions influencing the size, morphology, nucleation density and quality of the crystals were optimized. Highly transparent single crystals of average size 3 mm × 2 mm × 1 mm with well-defined hexagonal morphology were grown during a time period of two weeks. X-ray powder diffraction analysis revealed that the grown crystals crystallize in the monoclinic system with space group P21/c as identical with the pure cerium oxalate. The various functional groups of the oxalate ligand and the water of crystallization were identified by Fourier transform infrared spectroscopy. The photoluminescence spectrum of the Sm3+ doped cerium oxalate indicated that the Sm3+ ions are optically active in the cerium oxalate matrix. The crystal has a strong and efficient orange red emission with a wavelength peak at 595 nm and hence can be effectively used for optical amplification. Microhardness measurements of the crystal revealed that they belong to the soft material category.

  15. Production and several properties of single crystal austenitic stainless steels

    International Nuclear Information System (INIS)

    Okamoto, Kazutaka; Yoshinari, Akira; Kaneda, Junya; Aono, Yasuhisa; Kato, Takahiko

    1998-01-01

    The single crystal austenitic stainless steels Type 316L and 304L were grown in order to improve the resistance to stress corrosion cracking (SCC) using a unidirectional solidification method which can provide the large size single crystals. The mechanical properties and the chemical properties were examined. The orientation and temperature dependence of tensile properties of the single crystals were measured. The yield stress of the single crystal steels are lower than those of the conventional polycrystal steels because of the grain boundary strength cannot be expected in the single crystal steels. The tensile properties of the single crystal austenitic stainless steel Type 316L depend strongly on the orientation. The tensile strength in orientation are about 200 MPa higher than those in the and orientations. The microstructure of the single crystal consists of a mixture of the continuous γ-austenitic single crystal matrix and the δ-ferrite phase so that the effects of the γ/δ boundaries on the chemical properties were studied. The effects of the δ-ferrite phases and the γ/δ boundaries on the resistance to SCC were examined by the creviced bent beam test (CBB test). No crack is observed in all the CBB test specimens of the single crystals, even at the γ/δ boundaries. The behavior of the radiation induced segregation (RIS) at the γ/δ boundaries in the single crystal austenitic stainless steel Type 316L was evaluated by the electron irradiation test in the high voltage electron microscope (HVEM). The depletion of oversized solute chromium at the γ/δ boundary in the single crystal austenitic stainless steel Type 316L is remarkably lower than that at the grain boundary in the polycrystalline-type 316L. (author)

  16. Temperature effect on phase states of quartz nano-crystals in silicon single crystal

    International Nuclear Information System (INIS)

    Kalanov, M.U.; Ibragimova, E.M.; Khamraeva, R.N.; Rustamova, V.M.; Ummatov, Kh.D.

    2006-01-01

    Full text: Oxygen penetrates into the silicon lattice up to the concentration of 2·10 18 cm -3 in the course of growing [1]. By the author's opinion at a low oxygen content the formation of solid solution is possible in the local defect places of the silicon single crystal lattice due to the difference in effective ion radius of oxygen and silicon (r O 0.176 and r Si = 0.065 nm). Upon reaching some critical content (∼ 10 17 cm -3 ), it becomes favorable energetically for oxygen ions to form precipitates (SiO x ) and finally a dielectric layer (stoichiometric inclusions of SiO 2 ). It was shown later that depending on the growth conditions, indeed the quartz crystal inclusions are formed in the silicon single crystals at an amount of 0.3 /0.5 wt. % [2]. However the authors did not study a phase state of the quartz inclusions. Therefore the aim of this work was to study a phase state of the quartz inclusions in silicon crystal at various temperatures. We examined the silicon single crystals grown by Czochralski technique, which were cut in (111) plane in the form of disk of 20 mm diameter and 1.5 thickness and had hole conductivity with the specific resistance ρ o ≅ 1/10 Ohm cm. The dislocation density was N D ≅ 10 1 /10 3 cm -2 , the concentrations of oxygen and boron were N 0 ≅ 2/ 4·10 17 cm -3 and N B ≅ 3*10 15 cm -3 . Structure was analyzed at the set-up DRON-UM1 with high temperature supply UVD-2000 ( CuK = 0.1542 nm) at the temperatures of 300, 1173 and 1573 K measured with platinum-platinum-rhodium thermocouple. The high temperature diffraction spectrum measured at 1573 K in the angle range (2Θ≅10/70 d egree ) there is only one main structure reflection (111) with a high intensity and d/n ≅ 0.3136 nm (2 Θ≅ 28.5 d egree ) from the matrix lattice of silicon single crystal. The weak line at 2 Θ≅ 25.5 d egree ( d/n≅0.3136 nm) is β component of the main reflection (111), and the weak structure peak at 2Θ≅59 d egree ( d/n≅ 0.1568 nm

  17. Effect of amaranth on dielectric, thermal and optical properties of KDP single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Chandran, Senthilkumar; Paulraj, Rajesh, E-mail: rajeshp@ssn.edu.in; Ramasamy, P.

    2017-01-15

    Bulk single crystals of pure and amaranth doped KDP were grown using point seed technique. Effect of amaranth doping on KDP crystals was analyzed using powder XRD, thermal analysis (TG/DTA), dielectric, photoconductivity and etching studies. The phase purity and crystallinity of pure and dye doped crystals were confirmed by powder X-ray diffraction analysis. It is observed from TG-DTA analysis that the decomposition point decreased while doping with amaranth. Dielectric constant and loss increases with increasing temperatures. The photoconductivity decreases with the increase of amaranth concentration. - Highlights: • Pure and amaranth doped KDP crystals grown from point seed technique. • The addition of amaranth changes the decomposition points of dye doped KDP crystals. • Dielectric constant is increased. • It shows positive photoconductivity.

  18. Synthesis of formamidinium lead iodide perovskite bulk single crystal and its optical properties

    Science.gov (United States)

    Zheng, Hongge; Duan, Junjie; Dai, Jun

    2017-07-01

    Formamidinium lead iodide (FAPbI3) is a promising hybrid perovskite material for optoelectronic devices. We synthesized bulk single crystal FAPbI3 by a rapid solution crystallization method. X-ray diffraction (XRD) was performed to characterize the crystal structure. Temperature-dependent photoluminescence (PL) spectra of the bulk single crystal FAPbI3 were measured from 10 to 300 K to explain PL recombination mechanism. It shows that near band edge emission blueshifts with the temperature increasing from 10 to 120 K and from 140 K to room temperature, a sudden emission band redshift demonstrates near 140 K because of the phase transition from orthorhombic phase to cubic phase. From the temperature-dependent PL spectra, the temperature coefficients of the bandgap and thermal activation energies of FAPbI3 perovskite are fitted.

  19. Studies on the structural, optical and dielectric properties of samarium coordinated with salicylic acid single crystal

    Science.gov (United States)

    Singh, Harjinder; Slathia, Goldy; Gupta, Rashmi; Bamzai, K. K.

    2018-04-01

    Samarium coordinated with salicylic acid was successfully grown as a single crystal by low temperature solution technique using mixed solvent of methanol and water in equal ratio. Structural characterization was carried out by single crystal X-ray diffraction analysis and it crystallizes in centrosymmetric space group P121/c1. FTIR and UV-Vis-NIR spectroscopy confirmed the compound formation and help to determine the mode of binding of the ligand to the rare earth-metal ion. Dielectric constant and dielectric loss have been measured over the frequency range 100 Hz - 30MHz. The decrease in dielectric constant with increases in frequency is due to the transition from interfacial polarization to dipolar polarization. The small value of dielectric constant at higher frequency ensures that the crystal is good candidate for NLO devices. Dielectric loss represents the resistive nature of the material.

  20. Humidity control and hydrophilic glue coating applied to mounted protein crystals improves X-ray diffraction experiments

    Science.gov (United States)

    Baba, Seiki; Hoshino, Takeshi; Ito, Len; Kumasaka, Takashi

    2013-01-01

    Protein crystals are fragile, and it is sometimes difficult to find conditions suitable for handling and cryocooling the crystals before conducting X-ray diffraction experiments. To overcome this issue, a protein crystal-mounting method has been developed that involves a water-soluble polymer and controlled humid air that can adjust the moisture content of a mounted crystal. By coating crystals with polymer glue and exposing them to controlled humid air, the crystals were stable at room temperature and were cryocooled under optimized humidity. Moreover, the glue-coated crystals reproducibly showed gradual transformations of their lattice constants in response to a change in humidity; thus, using this method, a series of isomorphous crystals can be prepared. This technique is valuable when working on fragile protein crystals, including membrane proteins, and will also be useful for multi-crystal data collection. PMID:23999307

  1. The role of crystal orientation and surface proximity in the self-similar behavior of deformed Cu single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Pang, Judy W.L., E-mail: pangj@ornl.gov [Materials Science and Technology Division, Oak Ridge National Laboratory, 1 Behtel Valley Road, Oak Ridge, TN 37831 (United States); Ice, Gene E. [Materials Science and Technology Division, Oak Ridge National Laboratory, 1 Behtel Valley Road, Oak Ridge, TN 37831 (United States); Liu Wenjun [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2010-11-25

    We report on novel 3D spatially resolved X-ray diffraction microscopy studies of self-affine behavior in deformed single crystals. This study extends surface profile measurements of self-affined morphology changes in single crystals during deformation to include local lattice rotations and sub-surface behavior. Investigations were made on the spatial correlation of the local lattice rotations in 8% tensile deformed Cu single crystals oriented with [1 2 3], [1 1 1] and [0 0 1] axes parallel to the tensile axis. The nondestructive depth-resolved measurements were made over a length scale of one to hundreds of micrometers. Self-affined correlation was found both at the surface and below the surface of the samples. A universal exponent for the power-law similar to that observed with surface profile methods is found at the surface of all samples but crystallographically sensitive changes are observed as a function of depth. Correlation lengths of the self-affine behavior vary with the [1 2 3] crystal exhibiting the longest self-affine length scale of 70 {mu}m with only 18 {mu}m for the [1 1 1] and [0 0 1] crystals. These measurements illuminate the transition from surface-like to bulk-like deformation behavior and provide new quantitative information to guide emerging models of self-organized structures in plasticity.

  2. How far could energy transport within a single crystal

    Science.gov (United States)

    Zhang, Yifan; Che, Yanke; Zhao, Jincai; Steve, Granick

    Efficient transport of excitation energy over long distance is a vital process in light-harvesting systems and molecular electronics. The energy transfer distance is largely restricted by the probability decay of the exciton when hopping within a single crystal. Here, we fabricated an organic single crystal within which the energy could transfer more than 100 μm, a distance only limited by its crystal size. Our system could be regarded as a ``Sprint relay game'' performing on different surface of tracks. Photoinduced ``athletes'' (excitons) triggered intermolecular ``domino'' reaction to propagate energy for a long distance. In addition, athletes with the same ability runs much farther on smooth ideal track (single crystal assembled from merely van der Waals interaction) than bumpy mud track (crystal assembled from combination of pi-stacking, hydrogen bond and van der Waals interactions). Our finding presents new physics on enhancing energy transfer length within a single crystal. Current Affiliation: Institute for Basic Science, South Korea.

  3. Bulk crystal growth and nonlinear optical characterization of semiorganic single crystal: Cadmium (II) dibromide L - Proline monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Balakrishnan, T., E-mail: balacrystalgrowth@gmail.com [Crystal Growth Laboratory, PG & Research Department of Physics, Periyar EVR College (Autonomous), Tiruchirappalli, 620 023, Tamil Nadu (India); Sathiskumar, S. [Crystal Growth Laboratory, PG & Research Department of Physics, Periyar EVR College (Autonomous), Tiruchirappalli, 620 023, Tamil Nadu (India); Ramamurthi, K. [Crystal Growth and Thin Film Laboratory, Department of Physics and Nanotechnology, SRM University, Kattankulathur, 603 203, Kancheepuram, Tamil Nadu (India); Thamotharan, S. [Department of Bioinformatics, School of Chemical and Biotechnology, SASTRA University, Thanjavur, 613 401 (India)

    2017-01-15

    Single crystal of a novel metal organic nonlinear optical (NLO) cadmium (II) dibromide L - proline monohydrate (CBLPM) of size 7 × 7 × 5 mm{sup 3} was grown from slow evaporation technique. Single crystal X – ray diffraction analysis reveals that the crystal belongs to orthorhombic system with lattice parameters a = 10.1891 (8) Å, b = 13.4961 (11) Å, c = 7.4491 (5) Å and space group P2{sub 1}2{sub 1}2{sub 1}. The powder X – ray diffraction pattern of CBLPM was recorded and the X – ray diffraction peaks were indexed. The various functional groups of CBLPM were identified by the FT – IR and FT – Raman spectral analyses. The optical transmittance window and lower cut off wavelength of CBLPM were identified from UV – Vis – NIR studies. The mechanical strength of the grown crystal was estimated using Vickers microhardness test. Dielectric constant and dielectric loss measurements were carried out at different temperatures in the frequency range of 50 Hz - 2 MHz. The photoluminescence spectrum was recorded in the wavelength range 200–400 nm and the estimated optical band gap was ∼4.1 eV. Etching studies were carried out for different etching time. Thermal stability of CBLPM was determined using thermogravimetric analysis. Laser induced damage threshold study was carried out for the grown crystal using Nd:YAG laser. Size dependent second harmonic generation efficiency of the grown crystal was determined by Kurtz and Perry powder technique with different particle size using Nd:YAG laser with wavelength 1064 nm. Second harmonic generation efficiency of the powdered CBLPM crystal was ∼2.3 times that of potassium dihydrogen orthophosphate. - Highlights: • CBLPM crystal belongs to orthorhombic crystal system with space group P2{sub 1}2{sub 1}2{sub 1.} • Transmittance of CBLPM is ∼80% in the 650–1100 nm range. • Powder SHG efficiency of CBLPM increases with increase in particle size. • SHG efficiency of 0.57 μm size powdered CBLPM is ∼2

  4. Thermomechanical fatigue in single crystal superalloys

    Directory of Open Access Journals (Sweden)

    Moverare Johan J.

    2014-01-01

    Full Text Available Thermomechanical fatigue (TMF is a mechanism of deformation which is growing in importance due to the efficiency of modern cooling systems and the manner in which turbines and associated turbomachinery are now being operated. Unfortunately, at the present time, relatively little research has been carried out particularly on TMF of single crystal (SX superalloys, probably because the testing is significantly more challenging than the more standard creep and low cycle fatigue (LCF cases; the scarcity and relative expense of the material are additional factors. In this paper, the authors summarise their experiences on the TMF testing of SX superalloys, built up over several years. Emphasis is placed upon describing: (i the nature of the testing method, the challenges involved in ensuring that an given testing methodology is representative of engine conditions (ii the behaviour of a typical Re-containing second generation alloy such as CMSX-4, and its differing performance in out-of-phase/in-phase loading and crystallographic orientation and (iii the differences in behaviour displayed by the Re-containing alloys and new Re-free variants such as STAL15. It is demonstrated that the Re-containing superalloys are prone to different degradation mechanisms involving for example microtwinning, TCP precipitation and recrystallisation. The performance of STAL15 is not too inferior to alloys such as CMSX-4, suggesting that creep resistance itself does not correlate strongly with resistance to TMF. The implications for alloy design efforts are discussed.

  5. Magnetoresistance in terbium and holmium single crystals

    International Nuclear Information System (INIS)

    Singh, R.L.; Jericho, M.H.; Geldart, D.J.W.

    1976-01-01

    The longitudinal magnetoresistance of single crystals of terbium and holmium metals in their low-temperature ferromagnetic phase has been investigated in magnetic fields up to 80 kOe. Typical magnetoresistance isotherms exhibit a minimum which increases in depth and moves to higher fields as the temperature increases. The magnetoresistance around 1 0 K, where inelastic scattering is negligible, has been interpreted as the sum of a negative contribution due to changes in the domain structure and a positive contribution due to normal magnetoresistance. At higher temperatures, a phenomenological approach has been developed to extract the inelastic phonon and spin-wave components from the total measured magnetoresistance. In the temperature range 4--20 0 K (approximately), the phonon resistivity varies as T 3 . 7 for all samples. Approximate upper and lower bounds have been placed on the spin-wave resistivity which is also found to be described by a simple power law in this temperature range. The implications of this result for theoretical treatments of spin-wave resistivity due to s-f exchange interactions are considered. It is concluded that the role played by the magnon energy gap is far less transparent than previously suggested

  6. Solid-state molecular organometallic chemistry. Single-crystal to single-crystal reactivity and catalysis with light hydrocarbon substrates.

    Science.gov (United States)

    Chadwick, F Mark; McKay, Alasdair I; Martinez-Martinez, Antonio J; Rees, Nicholas H; Krämer, Tobias; Macgregor, Stuart A; Weller, Andrew S

    2017-08-01

    Single-crystal to single-crystal solid/gas reactivity and catalysis starting from the precursor sigma-alkane complex [Rh(Cy 2 PCH 2 CH 2 PCy 2 )(η 2 η 2 -NBA)][BAr F 4 ] (NBA = norbornane; Ar F = 3,5-(CF 3 ) 2 C 6 H 3 ) is reported. By adding ethene, propene and 1-butene to this precursor in solid/gas reactions the resulting alkene complexes [Rh(Cy 2 PCH 2 CH 2 PCy 2 )(alkene) x ][BAr F 4 ] are formed. The ethene ( x = 2) complex, [Rh(Cy 2 PCH 2 CH 2 PCy 2 )(ethene) 2 ][BAr F 4 ]-Oct , has been characterized in the solid-state (single-crystal X-ray diffraction) and by solution and solid-state NMR spectroscopy. Rapid, low temperature recrystallization using solution methods results in a different crystalline modification, [Rh(Cy 2 PCH 2 CH 2 PCy 2 )(ethene) 2 ][BAr F 4 ]-Hex , that has a hexagonal microporous structure ( P 6 3 22). The propene complex ( x = 1) [Rh(Cy 2 PCH 2 CH 2 PCy 2 )(propene)][BAr F 4 ] is characterized as having a π-bound alkene with a supporting γ-agostic Rh···H 3 C interaction at low temperature by single-crystal X-ray diffraction, variable temperature solution and solid-state NMR spectroscopy, as well as periodic density functional theory (DFT) calculations. A fluxional process occurs in both the solid-state and solution that is proposed to proceed via a tautomeric allyl-hydride. Gas/solid catalytic isomerization of d 3 -propene, H 2 C 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 0000000000000000000000000000000000 1111111111111111111111111111111111 1111111111111111111111111111111111

  7. Crystallization and diffraction analysis of the SARS coronavirus nsp10–nsp16 complex

    International Nuclear Information System (INIS)

    Debarnot, Claire; Imbert, Isabelle; Ferron, François; Gluais, Laure; Varlet, Isabelle; Papageorgiou, Nicolas; Bouvet, Mickaël; Lescar, Julien; Decroly, Etienne; Canard, Bruno

    2011-01-01

    The expression, purification and crystallization of the SARS coronavirus nsp16 RNA-cap AdoMet-dependent (nucleoside-2′O)-methyltransferase in complex with its activating factor nsp10 are reported. To date, the SARS coronavirus is the only known highly pathogenic human coronavirus. In 2003, it was responsible for a large outbreak associated with a 10% fatality rate. This positive RNA virus encodes a large replicase polyprotein made up of 16 gene products (nsp1–16), amongst which two methyltransferases, nsp14 and nsp16, are involved in viral mRNA cap formation. The crystal structure of nsp16 is unknown. Nsp16 is an RNA-cap AdoMet-dependent (nucleoside-2′-O-)-methyltransferase that is only active in the presence of nsp10. In this paper, the expression, purification and crystallization of nsp10 in complex with nsp16 are reported. The crystals diffracted to a resolution of 1.9 Å resolution and crystal structure determination is in progress

  8. Crystallization and preliminary X-ray diffraction studies of FAD synthetase from Corynebacterium ammoniagenes

    International Nuclear Information System (INIS)

    Herguedas, Beatriz; Martínez-Júlvez, Marta; Frago, Susana; Medina, Milagros; Hermoso, Juan A.

    2009-01-01

    Native and selenomethionine-labelled FAD synthetase from C. ammoniagenes have been crystallized by the hanging-drop vapour-diffusion method. A MAD data set for SeMet-labelled FAD synthetase was collected to 2.42 Å resolution, while data sets were collected to 1.95 Å resolution for the native crystals. FAD synthetase from Corynebacterium ammoniagenes (CaFADS), a prokaryotic bifunctional enzyme that catalyses the phosphorylation of riboflavin as well as the adenylylation of FMN, has been crystallized using the hanging-drop vapour-diffusion method at 277 K. Diffraction-quality cubic crystals of native and selenomethionine-labelled (SeMet-CaFADS) protein belonged to the cubic space group P2 1 3, with unit-cell parameters a = b = c = 133.47 Å and a = b = c = 133.40 Å, respectively. Data sets for native and SeMet-containing crystals were collected to 1.95 and 2.42 Å resolution, respectively

  9. Czochralski method of growing single crystals. State-of-art

    International Nuclear Information System (INIS)

    Bukowski, A.; Zabierowski, P.

    1999-01-01

    Modern Czochralski method of single crystal growing has been described. The example of Czochralski process is given. The advantages that caused the rapid progress of the method have been presented. The method limitations that motivated the further research and new solutions are also presented. As the example two different ways of the technique development has been described: silicon single crystals growth in the magnetic field; continuous liquid feed of silicon crystals growth. (author)

  10. LASER PROCESSING ON SINGLE CRYSTALS BY UV PULSE LASER

    OpenAIRE

    龍見, 雅美; 佐々木, 徹; 高山, 恭宜

    2009-01-01

    Laser processing by using UV pulsed laser was carried out on single crystal such as sapphire and diamond in order to understand the fundamental laser processing on single crystal. The absorption edges of diamond and sapphire are longer and shorter than the wave length of UV laser, respectively. The processed regions by laser with near threshold power of processing show quite different state in each crystal.

  11. Azeotropic binary solvent mixtures for preparation of organic single crystals

    NARCIS (Netherlands)

    Li, X.; Kjellander, B.K.C.; Anthony, J.E.; Bastiaansen, C.W.M.; Broer, D.J.; Gelinck, G.H.

    2009-01-01

    Here, a new approach is introduced to prepare large single crystals of π-conjugated organic molecules from solution. Utilizing the concept of azeotropism, single crystals of tri-isopropylsilylethynyl pentacene (TIPS-PEN) with dimensions up to millimeters are facilely self-assembled from homogeneous

  12. Azeotropic binary solvent mixtures for preparation of organic single crystals

    NARCIS (Netherlands)

    Li, X.; Kjellander, B.K.C.; Anthony, J.E.; Bastiaansen, C.W.M.; Broer, D.J.; Gelinck, G.H.

    2009-01-01

    Here, a new approach is introduced to prepare large single crystals of p-conjugated organic molecules from solution. Utilizing the concept of azeotropism, single crystals of tri-isopropylsilylethynyl pentacene (TIPS-PEN) with dimensions up to millimeters are facilely self-assembled from homogeneous

  13. Ion beam synthesis of buried single crystal erbium silicide

    International Nuclear Information System (INIS)

    Golanski, A.; Feenstra, R.; Galloway, M.D.; Park, J.L.; Pennycook, S.J.; Harmon, H.E.; White, C.W.

    1990-01-01

    High doses (10 16 --10 17 /cm 2 ) of 170 keV Er + were implanted into single-crystal left-angle 111 right-angle Si at implantation temperatures between 350 degree C and 520 degree C. Annealing at 800 degree C in vacuum following the implant, the growth and coalescence of ErSi 2 precipitates leads to a buried single crystalline ErSi 2 layer. This has been studied using Rutherford backscattering/channeling, X-ray diffraction, cross-sectional TEM and resistance versus temperature measurements. Samples implanted at 520 degree C using an Er dose of 7 x 10 16 /cm 2 and thermally annealed were subsequently used as seeds for the mesoepitaxial growth of the buried layer during a second implantation and annealing process. Growth occurs meso-epitaxially along both interfaces through beam induced, defect mediated mobility of Er atoms. The crystalline quality of the ErSi 2 layer strongly depends on the temperature during the second implantation. 12 refs., 4 figs

  14. A possibility of parallel and anti-parallel diffraction measurements on neu- tron diffractometer employing bent perfect crystal monochromator at the monochromatic focusing condition

    Science.gov (United States)

    Choi, Yong Nam; Kim, Shin Ae; Kim, Sung Kyu; Kim, Sung Baek; Lee, Chang-Hee; Mikula, Pavel

    2004-07-01

    In a conventional diffractometer having single monochromator, only one position, parallel position, is used for the diffraction experiment (i.e. detection) because the resolution property of the other one, anti-parallel position, is very poor. However, a bent perfect crystal (BPC) monochromator at monochromatic focusing condition can provide a quite flat and equal resolution property at both parallel and anti-parallel positions and thus one can have a chance to use both sides for the diffraction experiment. From the data of the FWHM and the Delta d/d measured on three diffraction geometries (symmetric, asymmetric compression and asymmetric expansion), we can conclude that the simultaneous diffraction measurement in both parallel and anti-parallel positions can be achieved.

  15. Crystallization and preliminary X-ray diffraction studies of l-rhamnose isomerase from Pseudomonas stutzeri

    International Nuclear Information System (INIS)

    Yoshida, Hiromi; Wayoon, Poonperm; Takada, Goro; Izumori, Ken; Kamitori, Shigehiro

    2006-01-01

    Recombinant l-rhamnose isomerase from P. stutzeri has been crystallized. Diffraction data have been collected to 2.0 Å resolution. l-Rhamnose isomerase from Pseudomonas stutzeri (P. stutzeril-RhI) catalyzes not only the reversible isomerization of l-rhamnose to l-rhamnulose, but also isomerization between various rare aldoses and ketoses. Purified His-tagged P. stutzeril-RhI was crystallized by the hanging-drop vapour-diffusion method. The crystals belong to the monoclinic space group P2 1 , with unit-cell parameters a = 74.3, b = 104.0, c = 107.0 Å, β = 106.8°. Diffraction data have been collected to 2.0 Å resolution. The molecular weight of the purified P. stutzeril-RhI with a His tag at the C-terminus was confirmed to be 47.7 kDa by MALDI–TOF mass-spectrometric analysis and the asymmetric unit is expected to contain four molecules

  16. Overexpression, purification, crystallization and preliminary diffraction studies of the Protaminobacter rubrum sucrose isomerase SmuA

    International Nuclear Information System (INIS)

    Ravaud, Stéphanie; Watzlawick, Hildegard; Haser, Richard; Mattes, Ralf; Aghajari, Nushin

    2005-01-01

    The P. rubrum sucrose isomerase SmuA, a key enzyme in the industrial production of isomaltulose, was crystallized and diffraction data were collected to 1.95 Å resolution. Palatinose (isomaltulose, α-d-glucosylpyranosyl-1,6-d-fructofuranose), a nutritional and acariogenic reducing sugar, is industrially obtained from sucrose by using immobilized cells of Protaminobacter rubrum that produce the sucrose isomerase SmuA. The isomerization of sucrose catalyzed by this enzyme also results in the formation of trehalulose (α-d-glucosylpyranosyl-1,1-d-fructofuranose) in smaller amounts and glucose, fructose and eventually isomaltose as by-products, which lower the yield of the reaction and complicate the recovery of palatinose. The determination of the three-dimensional structure of SmuA will provide a basis for rational protein-engineering studies in order to optimize the industrial production of palatinose. A recombinant form of the 67.3 kDa SmuA enzyme has been crystallized in the native state by the vapour-diffusion method. Crystals belong to the orthorhombic space group P2 1 2 1 2 1 , with unit-cell parameters a = 61.6, b = 81.4, c = 135.6 Å, and diffract to 1.95 Å resolution on a synchrotron-radiation source

  17. Crystallization and X-ray diffraction studies of crustacean proliferating cell nuclear antigen

    International Nuclear Information System (INIS)

    Carrasco-Miranda, Jesus S.; Cardona-Felix, Cesar S.; Lopez-Zavala, Alonso A.; Re Vega, Enrique de la; De la Mora, Eugenio; Rudiño-Piñera, Enrique; Sotelo-Mundo, Rogerio R.; Brieba, Luis G.

    2012-01-01

    Proliferating cell nuclear antigen from Litopenaeus vannamei was recombinantly expressed, purified and crystallized. Diffraction data were obtained and processed to 3 Å. Proliferating cell nuclear antigen (PCNA), a member of the sliding clamp family of proteins, interacts specifically with DNA replication and repair proteins through a small peptide motif called the PCNA-interacting protein or PIP box. PCNA is recognized as one of the key proteins involved in DNA metabolism. In the present study, the recombinant PCNA from Litopenaeus vannamei (LvPCNA) was heterologously overexpressed and purified using metal ion-affinity chromatography. Crystals suitable for diffraction grew overnight using the hanging-drop vapour-diffusion method. LvPCNA crystals belong to space group C2 with unit-cell parameters a = 144.6, b = 83.4, c = 74.3 Å, β = 117.6°. One data set was processed to 3 Å resolution, with an overall R meas of 0.09 and a completeness of 93.3%. Initial phases were obtained by molecular replacement using a homology model of LvPCNA as the search model. Refinement and structural analysis are underway. This report is the first successful crystallographic analysis of a marine crustacean decapod shrimp (L. vannamei) proliferating cell nuclear antigen

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

    Energy Technology Data Exchange (ETDEWEB)

    Boeshans, Karen M. [X-ray Crystallography Facility, NIAMS, National Institutes of Health, Bethesda, MD 20892 (United States); Wolf, Ronald; Voscopoulos, Christopher [Center for Cancer Research, National Cancer Institute, National Institutes of Health, Bethesda, MD 20892 (United States); Gillette, William; Esposito, Dominic [Protein Expression Laboratory, Research Technology Program, National Cancer Institute, SAIC-Frederick Inc., Frederick, MD 21702 (United States); Mueser, Timothy C. [Department of Chemistry, University of Toledo, Toledo, OH 43606 (United States); Yuspa, Stuart H. [Center for Cancer Research, National Cancer Institute, National Institutes of Health, Bethesda, MD 20892 (United States); Ahvazi, Bijan, E-mail: ahvazib@mail.nih.gov [X-ray Crystallography Facility, NIAMS, National Institutes of Health, Bethesda, MD 20892 (United States)

    2006-05-01

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

  19. Distributed Feedback Laser Based on Single Crystal Perovskite

    Science.gov (United States)

    Sun, Shang; Xiao, Shumin; Song, Qinghai

    2017-06-01

    We demonstrate a single crystal perovskite based, with grating-structured photoresist on top, highly polarized distributed feedback laser. A lower laser threshold than the Fabry-Perot mode lasers from the same single crystal CH3NH3PbBr3 microplate was obtained. Single crystal CH3NH3PbBr3 microplates was synthesized with one-step solution processed precipitation method. Once the photoresist on top of the microplate was patterned with electron beam, the device was realized. This one-step fabrication process utilized the advantage of single crystal to the greatest extend. The ultra-low defect density in single crystalline microplate offer an opportunity for lower threshold lasing action compare with poly-crystal perovskite films. In the experiment, the lasing action based on the distributed feedback grating design was found with lower threshold and higher intensity than the Fabry-Perot mode lasers supported by the flat facets of the same microplate.

  20. Structural, vibrational and thermal characterization of phase transformation in L-histidinium bromide monohydrate single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Moura, G.M. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Universidade Federal do Sul e Sudeste do Pará, ICEN, Marabá, PA 68505-080 (Brazil); Carvalho, J.O. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Instituto Federal do Tocantins, Araguaína, TO, 77.826-170 (Brazil); Silva, M.C.D.; Façanha Filho, P.F. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Santos, A.O. dos, E-mail: adenilson1@gmail.com [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil)

    2015-09-01

    L-Histidinium bromide monohydrate (LHBr) single crystal is a nonlinear optical material. In this work the high temperature phase transformation and the thermal stability of single crystals of LHBr was investigated by X-ray diffraction, thermogravimetric analysis, differential thermal analysis, differential scanning calorimetry and Raman spectroscopy. The results showed the LHBr phase transformation of orthorhombic (P2{sub 1}2{sub 1}2{sub 1}) to monoclinic system (P 1 2 1) at 120 °C, with the lattice parameters a = 12.162(1) Å, b = 16.821(2) Å, c = 19.477(2) Å and β = 108.56(2)°. These techniques are complementary and confirm the structural phase transformation due to loss water of crystallization. - Highlights: • -histidinium bromide single crystal was grown by slow evaporation technique. • X-ray diffraction characterize the high-temperature phase transformation. • The structural phase transformation occur due to loss of water of crystallization. • The LHBr thermal expansion coefficients exhibit an anisotropic behavior.

  1. Crystallinity of the epitaxial heterojunction of C60 on single crystal pentacene

    Science.gov (United States)

    Tsuruta, Ryohei; Mizuno, Yuta; Hosokai, Takuya; Koganezawa, Tomoyuki; Ishii, Hisao; Nakayama, Yasuo

    2017-06-01

    The structure of pn heterojunctions is an important subject in the field of organic semiconductor devices. In this work, the crystallinity of an epitaxial pn heterojunction of C60 on single crystal pentacene is investigated by non-contact mode atomic force microscopy and high-resolution grazing incidence x-ray diffraction. Analysis shows that the C60 molecules assemble into grains consisting of single crystallites on the pentacene single crystal surface. The in-plane mean crystallite size exceeds 0.1 μm, which is at least five time larger than the size of crystallites deposited onto polycrystalline pentacene thin films grown on SiO2. The results indicate that improvement in the crystal quality of the underlying molecular substrate leads to drastic promotion of the crystallinity at the organic semiconductor heterojunction.

  2. Crystallization and preliminary X-ray diffraction analysis of maize aldose reductase

    Energy Technology Data Exchange (ETDEWEB)

    Kiyota, Eduardo [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil); Centro de Biologia Molecular e Engenharia Genética, Universidade Estadual de Campinas, Campinas-SP (Brazil); Sousa, Sylvia Morais de [Centro de Biologia Molecular e Engenharia Genética, Universidade Estadual de Campinas, Campinas-SP (Brazil); Santos, Marcelo Leite dos; Costa Lima, Aline da [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil); Menossi, Marcelo [Departamento de Genética e Evolução, Instituto de Biologia, Universidade Estadual de Campinas, Campinas-SP (Brazil); Yunes, José Andrés [Laboratório de Biologia Molecular, Centro Infantil Boldrini, Campinas-SP (Brazil); Aparicio, Ricardo, E-mail: aparicio@iqm.unicamp.br [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil)

    2007-11-01

    Preliminary X-ray diffraction studies of apo maize aldose reductase at 2.0 Å resolution are reported. Maize aldose reductase (AR) is a member of the aldo-keto reductase superfamily. In contrast to human AR, maize AR seems to prefer the conversion of sorbitol into glucose. The apoenzyme was crystallized in space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 47.2, b = 54.5, c = 100.6 Å and one molecule in the asymmetric unit. Synchrotron X-ray diffraction data were collected and a final resolution limit of 2.0 Å was obtained after data reduction. Phasing was carried out by an automated molecular-replacement procedure and structural refinement is currently in progress. The refined structure is expected to shed light on the functional/enzymatic mechanism and the unusual activities of maize AR.

  3. Holographic Formation of Diffraction Elements for Transformation of Light Beams in Liquid Crystal - Photopolymer Compositions

    Science.gov (United States)

    Semkin, A. O.; Sharangovich, S. N.

    2018-03-01

    A theoretical model of holographic formation of diffractive optical elements for transformation of light beam field into Bessel-like fields in liquid crystal - photopolymer (LC-PPM) composite materials with a dyesensitizer is developed. Results of numerical modeling of kinetics ofvariation of the refractive index of a material in the process of formation with different relationships between the photopolymerization rates and diffusion processes are presented. Based on the results of numerical simulation, it is demonstrated that when the photopolarization process dominates, the diffractive element being formed is distorted. This leads to a change in the light field distribution at its output and consequently, to ineffective transformation of the reading beam. Thus, the necessity of optimizing of the recording conditions and of the prepolymeric composition to increase the transformation efficiency of light beam fields is demonstrated.

  4. Crystallization and preliminary X-ray diffraction analysis of maize aldose reductase

    International Nuclear Information System (INIS)

    Kiyota, Eduardo; Sousa, Sylvia Morais de; Santos, Marcelo Leite dos; Costa Lima, Aline da; Menossi, Marcelo; Yunes, José Andrés; Aparicio, Ricardo

    2007-01-01

    Preliminary X-ray diffraction studies of apo maize aldose reductase at 2.0 Å resolution are reported. Maize aldose reductase (AR) is a member of the aldo-keto reductase superfamily. In contrast to human AR, maize AR seems to prefer the conversion of sorbitol into glucose. The apoenzyme was crystallized in space group P2 1 2 1 2 1 , with unit-cell parameters a = 47.2, b = 54.5, c = 100.6 Å and one molecule in the asymmetric unit. Synchrotron X-ray diffraction data were collected and a final resolution limit of 2.0 Å was obtained after data reduction. Phasing was carried out by an automated molecular-replacement procedure and structural refinement is currently in progress. The refined structure is expected to shed light on the functional/enzymatic mechanism and the unusual activities of maize AR

  5. Reshock and release response of aluminum single crystal

    International Nuclear Information System (INIS)

    Huang, H.; Asay, J. R.

    2007-01-01

    Reshock and release experiments were performed on single crystal aluminum along three orientations and on polycrystalline 1050 aluminum with 50 μm grain size at shock stresses of 13 and 21 GPa to investigate the mechanisms for previously observed quasielastic recompression behavior. Particle velocity profiles obtained during reshocking both single crystals and polycrystalline aluminum from initial shock stresses of 13-21 GPa show similar quasielastic recompression behavior. Quasielastic release response is also observed in all single crystals, but the magnitude of the effect is crystal orientation dependent, with [111] and [110] exhibiting more ideal elastic-plastic release for unloading from the shocked state than for the [100] orientation and polycrystalline aluminum. The quasielastic response of 1050 aluminum is intermediate to that of the [100] and [111] orientations. Comparison of the wave profiles obtained for both unloading and reloading of single crystals and polycrystalline 1050 aluminum from shocked states suggests that the observed quasielastic response of polycrystalline aluminum results from the averaging response of single crystals for shock propagation along different orientations, and that the response of 1050 aluminum with large grain boundaries is not significantly different from the results obtained on single crystal aluminum. The yield strength of the single crystals and 1050 aluminum is found to increase with shock stress, which is consistent with previous results [H. Huang and I. R. Asay, J. Appl. Phys. 98, 033524 (2005)

  6. On the growth of calcium tartrate tetrahydrate single crystals

    Indian Academy of Sciences (India)

    2016-08-26

    Aug 26, 2016 ... The grown crystals were characterized by atomic absorption spectroscopy (AAS), X-ray diffraction analysis (XRD), microhardness measurement, Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG) and differential thermal analysis (DTA). The results obtained are compared with the ...

  7. Growth, optical, ICP and thermal studies of nonlinear optical single crystal: Sodium acid phthalate (NaAP)

    Science.gov (United States)

    Mahadevan, M.; Arivanandhan, M.; Elangovan, K.; Anandan, P.; Ramachandran, K.

    2017-07-01

    Good quality single crystals of sodium acid phthalate (NaAP) were grown by slow evaporation technique. Single crystal X-ray diffraction study of the grown crystal reveals that the crystal belongs to orthorhombic system with space group B2ab. Fourier transform infrared spectrum confirms the presence of the functional groups of the grown material. Inductively coupled plasma emission spectroscopy analysis is used to confirm the presence of Na element in the sample. Thermal analysis of the NaAP crystal shows that the crystal is stable up to 140°C. Optical transmittance of the grown crystal was recorded in the wavelength range from 200 and 800 nm using UV-Vis-NIR spectrophotometer. The second harmonic generation of NaAP was analysed using Kurtz powder technique.

  8. Crystallization and preliminary X-ray diffraction analysis of the CRISPR-Cas RNA-silencing Cmr complex.

    Science.gov (United States)

    Osawa, Takuo; Inanaga, Hideko; Numata, Tomoyuki

    2015-06-01

    Clustered regularly interspaced short palindromic repeat (CRISPR)-derived RNA (crRNA) and CRISPR-associated (Cas) proteins constitute a prokaryotic adaptive immune system (CRISPR-Cas system) that targets and degrades invading genetic elements. The type III-B CRISPR-Cas Cmr complex, composed of the six Cas proteins (Cmr1-Cmr6) and a crRNA, captures and cleaves RNA complementary to the crRNA guide sequence. Here, a Cmr1-deficient functional Cmr (CmrΔ1) complex composed of Pyrococcus furiosus Cmr2-Cmr3, Archaeoglobus fulgidus Cmr4-Cmr5-Cmr6 and the 39-mer P. furiosus 7.01-crRNA was prepared. The CmrΔ1 complex was cocrystallized with single-stranded DNA (ssDNA) complementary to the crRNA guide by the vapour-diffusion method. The crystals diffracted to 2.1 Å resolution using synchrotron radiation at the Photon Factory. The crystals belonged to the triclinic space group P1, with unit-cell parameters a = 75.5, b = 76.2, c = 139.2 Å, α = 90.3, β = 104.8, γ = 118.6°. The asymmetric unit of the crystals is expected to contain one CmrΔ1-ssDNA complex, with a Matthews coefficient of 2.03 Å(3) Da(-1) and a solvent content of 39.5%.

  9. Determination of Ni(II) crystal structure by powder x-ray diffraction ...

    African Journals Online (AJOL)

    X-ray powder diffraction pattern was used to determine the length of the unit cell, “a”, the lattice structure type, and the number of atoms per unit cell of Ni(II) crystal. The “a” value was determined to be 23.66 ± 0.005 Å, particle size of 34.87 nm, volume 13.24 Å and Strain value ε = 9.8 x 10-3. The cell search on PXRD patterns ...

  10. The Crystal Structure of the Malaria Pigment Hemozoin as Elucidated by X-ray Powder Diffraction

    DEFF Research Database (Denmark)

    Straasø, Tine

    survival. Successful inhibition of hemozoin crystallization will lead to parasitic death and thus break the cycle. The aim of this thesis is to elucidate the structure of hemozoin by means of X-ray diffraction techniques. Knowledge of the structure will help facilitate intelligent drug design in the future....... As part of the project an all-in-vacuum powder diffractometer was developed, which provides data with a minimum background level and an improved signal-to-noise ratio. Moreover, the diffractometer is designed with the particular purpose of decreasing the number of parameters to be fitted. Installation...

  11. High-quality bulk hybrid perovskite single crystals within minutes by inverse temperature crystallization

    KAUST Repository

    Saidaminov, Makhsud I.

    2015-07-06

    Single crystals of methylammonium lead trihalide perovskites (MAPbX3; MA=CH3NH3+, X=Br− or I−) have shown remarkably low trap density and charge transport properties; however, growth of such high-quality semiconductors is a time-consuming process. Here we present a rapid crystal growth process to obtain MAPbX3 single crystals, an order of magnitude faster than previous reports. The process is based on our observation of the substantial decrease of MAPbX3 solubility, in certain solvents, at elevated temperatures. The crystals can be both size- and shape-controlled by manipulating the different crystallization parameters. Despite the rapidity of the method, the grown crystals exhibit transport properties and trap densities comparable to the highest quality MAPbX3 reported to date. The phenomenon of inverse or retrograde solubility and its correlated inverse temperature crystallization strategy present a major step forward for advancing the field on perovskite crystallization.

  12. Excitonic polaritons of zinc diarsenide single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Syrbu, N.N., E-mail: sirbunn@yahoo.com [Technical University of Moldova, Chisinau, Republic of Moldova (Moldova, Republic of); Stamov, I.G. [T.G. Shevchenko State University of Pridnestrovie, Tiraspol, Republic of Moldova (Moldova, Republic of); Zalamai, V.V. [Institute of Applied Physics, Academy of Sciences of Moldova, Chisinau, Republic of Moldova (Moldova, Republic of); Dorogan, A. [Technical University of Moldova, Chisinau, Republic of Moldova (Moldova, Republic of)

    2017-02-01

    Excitonic polaritons of ZnAs{sub 2} single crystals had been investigated. Parameters of singlet excitons with Г{sub 2}¯(z) symmetry and orthoexcitons 2Г{sub 1}¯(y)+Г{sub 2}¯(x) had been determined. Spectral dependencies of ordinary and extraordinary dispersion of refractive index had been calculated using interferential reflection and transmittance spectra. It was shown, that A excitonic series were due to hole (V{sub 1}) and electron (C{sub 1}) bands. The values of effective masses of electrons (m{sub c}{sup *}=0.10 m{sub 0}) and holes (m{sub v1}{sup *}=0.89 m{sub 0}) had been estimated. It was revealed that the hole mass m{sub v1}{sup *} changes from 1.03 m{sub 0} to 0.55 m{sub 0} at temperature increasing from 10 K up to 230 K and that the electron mass m{sub c}{sup *} does not depend on temperature. The integral absorption A (eV cm{sup −1}) of the states n=1, 2 and 3 of Г{sub 2}¯(z) excitons depends on the A{sub n}≈n{sup −3} equality, which it is characteristic for S-type excitonic functions. Temperature dependences of the integral absorption of ground states for Г{sub 2}¯(z) and Г{sub 2}¯(Ñ…) excitons differ. The ground states of B and C excitons formed by V{sub 3} – C{sub 1} and V{sub 4} – C{sub 1} bands and its parameters had been determined.

  13. Anisotropic Light Diffraction by Ultrasound in Crystals with Strong Acoustic Anisotropy

    Science.gov (United States)

    Voloshin, Andrey S.; Balakshy, Vladimir I.

    In modern acousto-optics, crystalline materials are used predominantly for manufacturing acousto-optic instruments. Among these materials, such crystals as paratellurite, tellurium, calomel, TAS and some others occupy a prominent place, which are distinguished by exceptionally large anisotropy of acoustic properties. In this work, the influence of acoustic beam energy walk-off on characteristics of Bragg diffraction of light is studied by the example of tellurium crystal. It is shown that the walk-off can substantially change angular and frequency ranges, resulting in their narrowing or broadening subject to position of the operating point in the Bragg angle frequency characteristic. Coefficients of broadening are introduced for characterization of this effect.

  14. Super-broadband non-diffraction guiding modes in photonic crystals with elliptical rods

    Energy Technology Data Exchange (ETDEWEB)

    Liang, W Y; Wang, T B; Yin, C P; Dong, J W; Leng, F C; Wang, H Z, E-mail: stswhz@mail.sysu.edu.c [State Key Laboratory of Optoelectronic Materials and Technologies, Zhongshan (Sun Yat-Sen) University, Guangzhou 510275 (China)

    2010-02-24

    Non-diffraction guiding modes covering the full broad band of a photonic crystal with elliptical rods for TM mode are reported in this paper. All such modes can be used to effectively guide electromagnetic waves since they have near-zero group velocity components along the {Gamma}X' direction. In the fourth dispersion surface of the photonic crystal, the two wide flat regions spanning the first Brillouin zone possess unique properties: one dimension corresponds to a broad band, while the other corresponds to full incident angles of 0-90{sup 0}. These properties have many potential applications; as an example, here a broadband all-angle supercollimation with a bandwidth of 169 nm around 1550 nm is demonstrated. For the inverted structure of elliptical holes in a dielectric, similar results can be achieved over 140 nm around 1550 nm for TE mode.

  15. Crystallization and preliminary diffraction analysis of Wzi, a member of the capsule export and assembly pathway in Escherichia coli

    International Nuclear Information System (INIS)

    Bushell, Simon R.; Lou, Hubing; Wallat, Gregor D.; Beis, Konstantinos; Whitfield, Chris; Naismith, James H.

    2010-01-01

    Wzi is a membrane protein from E. coli thought to be involved in the attachment of capsular polysaccharides to the bacterial surface. This reports describes recombinant Wzi’s purification, crystallization and the results of initial diffraction studies. External polysaccharide capsules provide a physical barrier that is employed by many species of bacteria for the purposes of host evasion and persistence. Wzi is a 53 kDa outer membrane β-barrel protein that is thought to play a role in the attachment of group 1 capsular polysaccharides to the cell surface. The purification and crystallization of an Escherichia coli homologue of Wzi is reported and diffraction data from native and selenomethionine-incorporated protein crystals are presented. Crystals of C-terminally His 6 -tagged Wzi diffracted to 2.8 Å resolution. Data processing showed that the crystals belonged to the orthorhombic space group C222, with unit-cell parameters a = 128.8, b = 152.8, c = 94.4 Å, α = β = γ = 90°. A His-tagged selenomethionine-containing variant of Wzi has also been crystallized in the same space group and diffraction data have been recorded to 3.8 Å resolution. Data processing shows that the variant crystal has similar unit-cell parameters to the native crystal

  16. Purification, crystallization and preliminary X-ray diffraction of the G3BP1 NTF2-like domain

    DEFF Research Database (Denmark)

    Vognsen, Tina; Möller, Ingvar Rúnar; Kristensen, Ole

    2011-01-01

    The nuclear transport factor 2-like (NTF2-like) domain of human G3BP1 was subcloned, overexpressed in Escherichia coli and purified. Crystals were obtained using the hanging-drop vapour-diffusion method. Diffraction data were collected to 3.6 Å resolution using synchrotron radiation. The crystals...

  17. The structure of ultrathin iron films on tungsten single-crystal surfaces

    International Nuclear Information System (INIS)

    Gardiner, T.M.

    1983-01-01

    Ultrathin iron films vapour deposited onto the surface of a cylindrical tungsten single crystal are discussed. Results from work function change, Auger electron spectroscopic and low energy electron diffraction techniques are combined for a comparison of the initial stages of film growth on four low index planes. Advantage is taken of the opportunity to evaporate onto and simultaneously to make measurements on all surface orientations of the zone. (Auth.)

  18. Linear diffraction of light waves on periodically poled domain structures in lithium niobate crystals: collinear, isotropic, and anisotropic geometries

    International Nuclear Information System (INIS)

    Shandarov, S M; Mandel, A E; Akylbaev, T M; Borodin, M V; Savchenkov, E N; Smirnov, S V; Akhmatkhanov, A R; Shur, V Ya

    2017-01-01

    The possible variants of experimental observation of light diffraction on periodically poled domain structures (PPDS) in the lithium niobate crystal with 180-degree domain Y-walls are considered. We experimentally investigated isotropic and anisotropic diffraction of coherent light (λ = 655nm) on the PPDS with spatial period Λ = 8.79 μm produced by poling method in a LiNbO 3 : 5% MgO crystal. The central wavelength of irradiation experiencing a collinear diffraction on these PPDS is estimated as λ c = 455 nm. (paper)

  19. Prospects for the synthesis of large single-crystal diamonds

    International Nuclear Information System (INIS)

    Khmelnitskiy, R A

    2015-01-01

    The unique properties of diamond have stimulated the study of and search for its applications in many fields, including optics, optoelectronics, electronics, biology, and electrochemistry. Whereas chemical vapor deposition allows the growth of polycrystalline diamond plates more than 200 mm in diameter, most current diamond application technologies require large-size (25 mm and more) single-crystal diamond substrates or films suitable for the photolithography process. This is quite a challenge, because the largest diamond crystals currently available are 10 mm or less in size. This review examines three promising approaches to fabricating large-size diamond single crystals: growing large-size single crystals, the deposition of heteroepitaxial diamond films on single-crystal substrates, and the preparation of composite diamond substrates. (reviews of topical problems)

  20. Synthesis and structural characterization of bulk Sb2Te3 single crystal

    Science.gov (United States)

    Sultana, Rabia; Gahtori, Bhasker; Meena, R. S.; Awana, V. P. S.

    2018-05-01

    We report the growth and characterization of bulk Sb2Te3 single crystal synthesized by the self flux method via solid state reaction route from high temperature melt (850˚C) and slow cooling (2˚C/hour) of constituent elements. The single crystal X-ray diffraction pattern showed the 00l alignment and the high crystalline nature of the resultant sample. The rietveld fitted room temperature powder XRD revealed the phase purity and rhombohedral structure of the synthesized crystal. The formation and analysis of unit cell structure further verified the rhombohedral structure composed of three quintuple layers stacked one over the other. The SEM image showed the layered directional growth of the synthesized crystal carried out using the ZEISS-EVOMA-10 scanning electron microscope The electrical resistivity measurement was carried out using the conventional four-probe method on a quantum design Physical Property Measurement System (PPMS). The temperature dependent electrical resistivity plot for studied Sb2Te3 single crystal depicts metallic behaviour in the absence of any applied magnetic field. The synthesis as well as the structural characterization of as grown Sb2Te3 single crystal is reported and discussed in the present letter.

  1. The purification, crystallization and preliminary diffraction of a glycerophosphodiesterase from Enterobacter aerogenes

    International Nuclear Information System (INIS)

    Jackson, Colin J.; Carr, Paul D.; Kim, Hye-Kyung; Liu, Jian-Wei; Ollis, David L.

    2006-01-01

    The metallo-glycerophosphodiesterase from E. aerogenes (GpdQ) has been cloned, expressed in E. coli and purified. Initial screening of crystallization conditions for this enzyme resulted in the identification of needles from one condition in a sodium malonate grid screen. Removal of the metals from the enzyme and subsequent optimization of these conditions led to crystals. The metallo-glycerophosphodiesterase from Enterobacter aerogenes (GpdQ) has been cloned, expressed in Escherichia coli and purified. Initial screening of crystallization conditions for this enzyme resulted in the identification of needles from one condition in a sodium malonate grid screen. Removal of the metals from the enzyme and subsequent optimization of these conditions led to crystals that diffracted to 2.9 Å and belonged to space group P2 1 3, with unit-cell parameter a = 164.1 Å. Self-rotation function analysis and V M calculations indicated that the asymmetric unit contains two copies of the monomeric enzyme, corresponding to a solvent content of 79%. It is intended to determine the structure of this protein utilizing SAD phasing from transition metals or molecular replacement

  2. The purification, crystallization and preliminary diffraction of a glycerophosphodiesterase from Enterobacter aerogenes

    Energy Technology Data Exchange (ETDEWEB)

    Jackson, Colin J.; Carr, Paul D.; Kim, Hye-Kyung; Liu, Jian-Wei; Ollis, David L., E-mail: ollis@rsc.anu.edu.au [The Research School of Chemistry, Australian National University, ACT 0200 (Australia)

    2006-07-01

    The metallo-glycerophosphodiesterase from E. aerogenes (GpdQ) has been cloned, expressed in E. coli and purified. Initial screening of crystallization conditions for this enzyme resulted in the identification of needles from one condition in a sodium malonate grid screen. Removal of the metals from the enzyme and subsequent optimization of these conditions led to crystals. The metallo-glycerophosphodiesterase from Enterobacter aerogenes (GpdQ) has been cloned, expressed in Escherichia coli and purified. Initial screening of crystallization conditions for this enzyme resulted in the identification of needles from one condition in a sodium malonate grid screen. Removal of the metals from the enzyme and subsequent optimization of these conditions led to crystals that diffracted to 2.9 Å and belonged to space group P2{sub 1}3, with unit-cell parameter a = 164.1 Å. Self-rotation function analysis and V{sub M} calculations indicated that the asymmetric unit contains two copies of the monomeric enzyme, corresponding to a solvent content of 79%. It is intended to determine the structure of this protein utilizing SAD phasing from transition metals or molecular replacement.

  3. Purification, crystallization and preliminary X-ray diffraction studies on avian haemoglobin from pigeon (Columba livia)

    International Nuclear Information System (INIS)

    Sathya Moorthy, Pon.; Neelagandan, K.; Balasubramanian, M.; Ponnuswamy, M. N.

    2009-01-01

    Crystallization of pigeon haemoglobin at low pH (5.5) and high ionic concentration (1 M) using the hanging-drop vapour-diffusion method is reported. Haemoglobin is a physiologically significant metalloprotein that is involved in the exchange of gases for sustaining life. The respiratory system of birds is unique and complex compared with that of mammals. Many investigations of avian haemoglobins have revealed the presence of inositol pentaphosphate (IP5), a principal allosteric effector that is involved in regulation of their function. Structural investigations of avian haemoglobins are presently not adequate to explain their function. Efforts have been made in this direction in order to understand the oxygen-binding affinity involved in adapting to hypoxia in avian haemoglobins. Fresh whole blood was collected from pigeon (Columba livia) and purified using a DEAE cellulose anion-exchange chromatographic column. Crystallization of pigeon haemoglobin was accomplished using the hanging-drop vapour-diffusion method using PEG 3350 as a precipitant in 50 mM sodium acetate buffer pH 5.5 with 1 M NaCl. Data collection was carried out using a MAR345 image-plate detector system. The crystals diffracted to 2 Å resolution. Pigeon haemoglobin crystallizes in a triclinic space group, with two whole biological molecules in the asymmetric unit and with unit-cell parameters a = 55.005, b = 65.528, c = 104.370 Å, α = 78.742, β = 89.819, γ = 65.320°

  4. Expression, purification, crystallization and preliminary X-ray diffraction analysis of grass carp β2-microglobulin

    International Nuclear Information System (INIS)

    Chen, Weihong; Chu, Fuliang; Peng, Hao; Zhang, Jianhua; Qi, Jianxun; Jiang, Fan; Xia, Chun; Gao, Feng

    2008-01-01

    Grass carp β 2 -microglobulin was expressed in E. coli, purified to homogeneity and crystallized using the hanging-drop vapour-diffusion method with PEG 2K as precipitant. The crystals obtained belong to the orthorhombic space group P2 1 2 1 2 1 , with unit-cell parameters a = 38.72, b = 40.65, c = 71.12 Å. β 2 -Microglobulin (β 2 m) is an essential subunit of MHC I molecules; it stabilizes the structure of MHC I and plays a pivotal role in coreceptor recognition. To date, structures of β 2 m have been solved for three different mammals: human, mouse and cattle. In order to illuminate the molecular evolutionary origin of β2m, an understanding of its structure in lower vertebrates becomes important. Here, grass carp (Ctenopharyngodon idellus) β 2 m (Ctid-β 2 m) was expressed, purified and crystallized. Diffraction data were collected to a resolution of 2.5 Å. The crystal belongs to space group P2 1 2 1 2 1 , with unit-cell parameters a = 38.72, b = 40.65, c = 71.12 Å. The Matthews coefficient and the solvent content were calculated to be 2.56 Å Da −1 and 52.07%, respectively, for one molecule per asymmetric unit. The structure has been solved by molecular replacement using monomeric human β 2 m as a model

  5. Dynamic Diffraction Studies on the Crystallization, Phase Transformation, and Activation Energies in Anodized Titania Nanotubes

    Directory of Open Access Journals (Sweden)

    Hani Albetran

    2018-02-01

    Full Text Available The influence of calcination time on the phase transformation and crystallization kinetics of anodized titania nanotube arrays was studied using in-situ isothermal and non-isothermal synchrotron radiation diffraction from room temperature to 900 °C. Anatase first crystallized at 400 °C, while rutile crystallized at 550 °C. Isothermal heating of the anodized titania nanotubes by an increase in the calcination time at 400, 450, 500, 550, 600, and 650 °C resulted in a slight reduction in anatase abundance, but an increase in the abundance of rutile because of an anatase-to-rutile transformation. The Avrami equation was used to model the titania crystallization mechanism and the Arrhenius equation was used to estimate the activation energies of the titania phase transformation. Activation energies of 22 (10 kJ/mol for the titanium-to-anatase transformation, and 207 (17 kJ/mol for the anatase-to-rutile transformation were estimated.

  6. Purification, crystallization and preliminary X-ray diffraction of fluorescence recovery protein from Synechocystis PCC 6803

    International Nuclear Information System (INIS)

    Liu, Ting; Shuai, Yingli; Zhou, Honggang

    2011-01-01

    Fluorescence recovery protein from Synechocystis PCC 6803 plays a key role in the orange carotenoid protein-related photoprotective mechanism in cyanobacteria. The full-length form and a truncated form were overexpressed, purified and crystallized, and diffraction was observed to 2.75 Å resolution. Fluorescence recovery protein (FRP), which is encoded by the slr1964 gene in Synechocystis PCC 6803, plays a key role in the orange carotenoid protein-related photoprotective mechanism in cyanobacteria. As the crystal structure of FRP may provide information about the biological functions and mechanism of action of the protein, recombinant full-length FRP and a truncated form were overexpressed, purified and crystallized at 291 K using ethylene imine polymer as the precipitant. An FRP data set was collected to a resolution of 2.75 Å at low temperature (100 K). The crystal belonged to space group P4 1 2 1 2, with unit-cell parameters a = b = 61.9, c = 160.7 Å, α = β = γ = 90°. Assuming that the asymmetric unit contains three molecules, the Matthews coefficient was calculated to be 2.1 Å 3 Da −1

  7. Growth and dielectric, mechanical, thermal and etching studies of an organic nonlinear optical L-arginine trifluoroacetate (LATF) single crystal

    International Nuclear Information System (INIS)

    Arjunan, S.; Mohan Kumar, R.; Mohan, R.; Jayavel, R.

    2008-01-01

    L-arginine trifluoroacetate, an organic nonlinear optical material, has been synthesized from aqueous solution. Bulk single crystal of dimension 57 mm x 5 mm x 3 mm has been grown by temperature lowering technique. Powder X-ray diffraction studies confirmed the monoclinic structure of the grown L-arginine trifluoroacetate crystal. Linear optical property of the grown crystal has been studied by UV-vis spectrum. Dielectric response of the L-arginine trifluoroacetate crystal was analysed for different frequencies and temperatures in detail. Microhardness study on the sample reveals that the crystal possesses relatively higher hardness compared to many organic crystals. Thermal analyses confirmed that the L-arginine trifluoroacetate material is thermally stable upto 212 deg. C. The etching studies have been performed to assess the perfection of the L-arginine trifluoroacetate crystal. Kurtz powder second harmonic generation test confirms the nonlinear optical properties of the as-grown L-arginine trifluoroacetate crystal

  8. X-ray diffraction topography observations of the core in Bi12SiO20 crystals doped with Mn

    International Nuclear Information System (INIS)

    Milenov, T.I.; Botev, P.A.; Rafailov, P.M.; Gospodinov, M.M.

    2004-01-01

    The core region in a bismuth silicate--Bi 12 SiO 20 (BSO) crystal doped with Mn was examined by X-ray double-crystal diffraction topography. Specific features were observed in the topographies as lines and contrast differences that point to defects occupying the central part of the crystal. We discuss the nature of these defects and propose an explanation in terms of stacking faults arranged in different structures

  9. Crystallization and preliminary electron diffraction study to 3. 7 A of DNA helix-destabilizing protein gp32*I

    Energy Technology Data Exchange (ETDEWEB)

    Chiu, W; Hosoda, J

    1978-01-01

    A two-dimensionally large and thin crystal has been obtained from gp32*I, a proteolytically digested product of a DNA helix-destabilizing protein coded by gene 32 in bacteriophage T4. High-resolution electron diffraction patterns (approx. 3.7 A) are recorded from both unstained and stained protein crystals embedded in glucose. The crystal is of orthorhombic space group with a = 62.9 A and b = 47.3 A.

  10. Synthesis and growth of single crystals of PrCl3

    International Nuclear Information System (INIS)

    Pei, Jen Shieh.

    1984-01-01

    An efficient method for growth of high optical quality single crystals of PrCl 3 . The method consists in careful drying of the hydrated chloride, PrCl 3 . 7H 2 O, with a protective atmosphere of anhydrous HCl and Ar. A subsequent growth was done by the zone melting technique. The hydrated chloride had prepared from dissolution of the oxide Pr 6 O 11 in hydrochloric acid. The grown crystals had characterized fluorescence and x-ray diffraction measurements. (Author) [pt

  11. Single Crystal Growth of Pure Co3+ Oxidation State Material LaSrCoO4

    Directory of Open Access Journals (Sweden)

    Hanjie Guo

    2016-08-01

    Full Text Available We report on the single crystal growth of the single-layer perovskite cobaltate LaSrCoO4 that was grown by the optical floating zone method using high oxygen pressures. Phase purity and single crystallinity were confirmed by X-ray diffraction techniques. The pure Co3+ oxidation state was confirmed by X-ray absorbtion spectroscopy measurements. A transition to a spin glass state is observed at ∼7 K in magnetic susceptibility and specific heat measurements.

  12. Crystallization and preliminary X-ray diffraction studies of the tetramerization domain derived from the human potassium channel Kv1.3

    International Nuclear Information System (INIS)

    Winklmeier, Andreas; Weyand, Michael; Schreier, Christina; Kalbitzer, Hans Robert; Kremer, Werner

    2009-01-01

    The tetramerization domain of human Kv1.3 was cloned, expressed, purified and crystallized. The crystals belonged to space group I4 and diffracted to 1.2 Å resolution using synchrotron radiation. The tetramerization domain (T1 domain) derived from the voltage-dependent potassium channel Kv1.3 of Homo sapiens was recombinantly expressed in Escherichia coli and purified. The crystals were first grown in an NMR tube in 150 mM potassium phosphate pH 6.5 in the absence of additional precipitants. The crystals showed I4 symmetry characteristic of the naturally occurring tetrameric assembly of the single subunits. A complete native data set was collected to 1.2 Å resolution at 100 K using synchrotron radiation

  13. Ultra-large single crystals by abnormal grain growth.

    Science.gov (United States)

    Kusama, Tomoe; Omori, Toshihiro; Saito, Takashi; Kise, Sumio; Tanaka, Toyonobu; Araki, Yoshikazu; Kainuma, Ryosuke

    2017-08-25

    Producing a single crystal is expensive because of low mass productivity. Therefore, many metallic materials are being used in polycrystalline form, even though material properties are superior in a single crystal. Here we show that an extraordinarily large Cu-Al-Mn single crystal can be obtained by abnormal grain growth (AGG) induced by simple heat treatment with high mass productivity. In AGG, the sub-boundary energy introduced by cyclic heat treatment (CHT) is dominant in the driving pressure, and the grain boundary migration rate is accelerated by repeating the low-temperature CHT due to the increase of the sub-boundary energy. With such treatment, fabrication of single crystal bars 70 cm in length is achieved. This result ensures that the range of applications of shape memory alloys will spread beyond small-sized devices to large-scale components and may enable new applications of single crystals in other metallic and ceramics materials having similar microstructural features.Growing large single crystals cheaply and reliably for structural applications remains challenging. Here, the authors combine accelerated abnormal grain growth and cyclic heat treatments to grow a superelastic shape memory alloy single crystal to 70 cm.

  14. Structure of cleaved (001) USb2 single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Shao-ping [Los Alamos National Laboratory; Hawley, Marilyn [Los Alamos National Laboratory; Bauer, Eric D [Los Alamos National Laboratory; Stockum, Phil B [STANFORD UNIV.; Manoharan, Hari C [STANFORD UNIV

    2009-01-01

    We have achieved what we believe to be the first atomic resolution STM images for a uranium compound taken at room temperature. The a, b, and c lattice parameters in the images confirm that the USb{sub 2} crystals cleave on the (001) basal plane as expected. The a and b dimensions were equal, with the atoms arranged in a cubic pattern. Our calculations indicate a symmetric cut between Sb planes to be the most favorable cleavage plane and U atoms to be responsible for most of the DOS measured by STM. Some strange features observed in the STM will be discussed in conjunction with ab initio calculations. The purpose of this work is to demonstrate the power of scanning tunneling microscopy (STM) techniques combined with a theoretical underpinning to determine the surface atomic structure and properties of actinide materials, such as the quasi 2-dimensional uranium dipnictide USb{sub 2} single crystal, thereby contributing to the understanding of their surface structural and electronic properties. The members of this interesting UX{sub 2} (X=P, As, Sb, Bi) series of compounds display dual localized and itinerant 5f electron behavior within the same compound due to the hybridization of the 5f orbitals with the conduction band. With the exception of UO{sub 2}, which has to be studied at elevated temperature to generate enough carriers for STM imaging, STM techniques have not been applied successfully to the characterization of the surface atomic structure of any other single crystal actinide compound, to the best of our knowledge. However, STM has been used to a limited extent for the study of some cerium compounds. STM probes electronic properties at the atomic level and can directly provide information about the local density of filled and empty states (LDOS) states simultaneously. A STM topograph provides the local atomic arrangement and spacing of the atoms on the surface, local defect structures (e.g. steps, vacancies, and kink sites) and the presence of contaminants

  15. Crystallization and X-ray diffraction analysis of human CLEC5A (MDL-1), a dengue virus receptor

    International Nuclear Information System (INIS)

    Watson, Aleksandra A.; O’Callaghan, Christopher A.

    2009-01-01

    Recombinant human CLEC5A was crystallized in the trigonal space group P3 1 and X-ray diffraction data were collected to 1.56 Å resolution. The human C-type lectin-like protein CLEC5A (also known as MDL-1) is expressed on the surface of myeloid cells and plays a critical role in dengue-virus-induced disease by signalling through the transmembrane adaptor protein DAP12. The C-type lectin-like domain of CLEC5A was expressed in Escherichia coli, refolded and purified. Recombinant CLEC5A crystals were grown by sitting-drop vapour diffusion using polyethylene glycol 6000 as a precipitant. After optimization, crystals were grown which diffracted to 1.56 Å using synchrotron radiation. The results presented in this paper suggest that crystals producing diffraction of this quality will be suitable for structural determination of human CLEC5A

  16. Crystal growth, morphology, thermal and spectral studies of an organosulfur nonlinear optical bis(guanidinium) 5-sulfosalicylate (BG5SS) single crystals

    Science.gov (United States)

    Dhavamurthy, M.; Peramaiyan, G.; Babu, K. Syed Suresh; Mohan, R.

    2015-04-01

    Organosulfur nonlinear optical single crystals of orthorhombic bis(guanidinium) 5-sulfosalicylate (2CH6N3 +·C7H4O6S2-·H2O) with dimension 14 mm × 4 mm × 5 mm have been grown from methanol and water solvents in 1:1 ratio by the slow evaporation growth technique. The crystal structure and morphology of the crystals have been studied by single-crystal X-ray diffraction. FTIR spectroscopic studies were carried out to identify the functional groups and vibrational modes present in the grown crystals. The UV-Vis spectrum was studied to analyze the linear optical properties of the grown crystals. The thermal gravimetric analysis was conducted on the grown crystals, and the result revealed that the grown crystal is thermally stable up to 65 °C. The dielectric tensor components ɛ 11, ɛ 22 and ɛ 33 of BG5SS crystal were evaluated as a function of frequency at 40 °C. The surface laser damage threshold for the grown crystal was measured using Nd:YAG laser. Further, Vickers micro-hardness study was carried out to analyze the mechanical strength of the grown crystals for various loads.

  17. Time-Resolved Soft X-ray Diffraction Reveals Transient Structural Distortions of Ternary Liquid Crystals

    Directory of Open Access Journals (Sweden)

    Klaus Mann

    2009-11-01

    Full Text Available Home-based soft X-ray time-resolved scattering experiments with nanosecond time resolution (10 ns and nanometer spatial resolution were carried out at a table top soft X-ray plasma source (2.2–5.2 nm. The investigated system was the lyotropic liquid crystal C16E7/paraffin/glycerol/formamide/IR 5. Usually, major changes in physical, chemical, and/or optical properties of the sample occur as a result of structural changes and shrinking morphology. Here, these effects occur as a consequence of the energy absorption in the sample upon optical laser excitation in the IR regime. The liquid crystal shows changes in the structural response within few hundred nanoseconds showing a time decay of 182 ns. A decrease of the Bragg peak diffracted intensity of 30% and a coherent macroscopic movement of the Bragg reflection are found as a response to the optical pump. The Bragg reflection movement is established to be isotropic and diffusion controlled (1 μs. Structural processes are analyzed in the Patterson analysis framework of the time-varying diffraction peaks revealing that the inter-lamellar distance increases by 2.7 Å resulting in an elongation of the coherently expanding lamella crystallite. The present studies emphasize the possibility of applying TR-SXRD techniques for studying the mechanical dynamics of nanosystems.

  18. Crystal structure investigations on cation-substituted alums by X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Abdeen, A.M.

    1980-04-01

    The crystal structures of the three alums: NH 4 Al(SO 4 ) 2 .12H 2 O, (NH 3 CH 3 )Al(SO 4 ) 2 .12H 2 O and (NH 3 OH)Al(SO 4 ) 2 .12H 2 O have been determined from three-dimensional neutron diffraction data enhanced by X-ray diffraction when necessary. These compounds crystallize cubic in space group Pa3. The structures of the three alums exhibit partial occupancies of crystallographic sites for the NH 4 , (NH 3 CH 3 ) and (NH 3 OH) group atoms. This can be explained by a quantized rotation of the three groups around an axis perpendicular to the [111] direction. Some of the (SO 4 ) 2- groups in the NH 4 -alum are disordered with about 17% of the sulfate tetrahedra being in a reversed orientation around the sulfur atom. The disorder in (NH 3 CH 3 ) and (NH 3 OH)-alums is only 4,3% and 3.0% respectively. The atoms in the alum structures are held together by a system of hydrogen bonds between the water molecules and between the water molecules and the sulfate oxygen atoms. In these three structures there is a strong indication that shorter hydrogen bonds tend to be nearly linear. (orig.)

  19. Crystal chemistry of nephelines from ijolites and nepheline-rich pegmatites: influence of composition and genesis on the crystal structure investigated by X-ray diffraction

    DEFF Research Database (Denmark)

    Vulić, Predrag; Balić-Žunić, Tonči; Belmonte, Louise Josefine

    2011-01-01

    Ten nepheline single crystals from five different localities representing rocks from nepheline-syenite pegmatites to urtite, ijolite and cancrinite-ijolite were investigated chemically and structurally. The chemical compositions were determined by electron microprobe, whereas the crystal structur...

  20. Growth and characterization of LiInSe2 single crystals

    Science.gov (United States)

    Ma, Tianhui; Zhu, Chongqiang; Lei, Zuotao; Yang, Chunhui; Sun, Liang; Zhang, Hongchen

    2015-04-01

    Large and crack-free LiInSe2 single crystals were obtained by the vertical gradient freezing method with adding a temperature oscillation technology in a two-zone furnace. X-ray diffraction data showed that the pure LiInSe2 compound was synthesized. The grown crystals had different color depending on melt composition. The atomic ratios of elements of LiInSe2 crystals were obtained by an Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES), and the structural formula were calculated according to the relative contents of elements. The average absorption coefficients were estimated by using average reflection indices. The absorption coefficients of the thermal annealing samples are 0.6 cm-1 at 2-3 μm. The transparent range of our LiInSe2 crystals is from 0.6 μm to 13.5 μm.

  1. Effect of 120 MeV Ag{sup 9+} ion irradiation of YCOB single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Arun Kumar, R., E-mail: rarunpsgtech@yahoo.com [Crystal Growth Centre, Anna University, Chennai 600 025 (India); Department of Basic Sciences - Physics Division, PSG College of Technology, Coimbatore 641 004 (India); Dhanasekaran, R. [Crystal Growth Centre, Anna University, Chennai 600 025 (India)

    2012-09-15

    Single crystals of yttrium calcium oxy borate (YCOB) grown from boron-tri-oxide flux were subjected to swift heavy ion irradiation using silver Ag{sup 9+} ions from the 15 UD Pelletron facility at Inter University Accelerator Center, New Delhi. The crystals were irradiated at 1 Multiplication-Sign 10{sup 13}, 5 Multiplication-Sign 10{sup 13} and 1 Multiplication-Sign 10{sup 14} ions/cm{sup 2} fluences at room temperature and with 5 Multiplication-Sign 10{sup 13} ions/cm{sup 2} fluence at liquid nitrogen temperature. The pristine and the irradiated samples were characterized by glancing angle X-ray diffraction, UV-Vis-NIR and photoluminescence studies. From the characterization studies performed on the samples, it is inferred that the crystals irradiated at liquid nitrogen temperature had fewer defects compared to the crystals irradiated at room temperature and the defects increased when the ion fluence was increased at room temperature.

  2. Understanding surface structure and chemistry of single crystal lanthanum aluminate

    KAUST Repository

    Pramana, Stevin S.

    2017-03-02

    The surface crystallography and chemistry of a LaAlO3 single crystal, a material mainly used as a substrate to deposit technologically important thin films (e.g. for superconducting and magnetic devices), was analysed using surface X-ray diffraction and low energy ion scattering spectroscopy. The surface was determined to be terminated by Al-O species, and was significantly different from the idealised bulk structure. Termination reversal was not observed at higher temperature (600 °C) and chamber pressure of 10−10 Torr, but rather an increased Al-O occupancy occurred, which was accompanied by a larger outwards relaxation of Al from the bulk positions. Changing the oxygen pressure to 10−6 Torr enriched the Al site occupancy fraction at the outermost surface from 0.245(10) to 0.325(9). In contrast the LaO, which is located at the next sub-surface atomic layer, showed no chemical enrichment and the structural relaxation was lower than for the top AlO2 layer. Knowledge of the surface structure will aid the understanding of how and which type of interface will be formed when LaAlO3 is used as a substrate as a function of temperature and pressure, and so lead to improved design of device structures.

  3. Spherical Nb single crystals containerlessly grown by electrostatic levitation

    International Nuclear Information System (INIS)

    Sung, Y.S.; Takeya, H.; Hirata, K.; Togano, K.

    2003-01-01

    Spherical Nb (T m =2750 K) single crystals were grown via containerless electrostatic levitation (ESL). Samples became spherical at melting in levitation and undercooled typically 300-450 K prior to nucleation. As-processed samples were still spherical without any macroscopic shape change by solidification showing a uniform dendritic surface morphology. Crystallographic {111} planes exposed in equilateral triangular shapes on the surface by preferential macroetching and spotty back-reflection Laue patterns confirm the single crystal nature of the ESL-processed Nb samples. No hysteresis in magnetization between zero field and field cooling also implies a clean defect-free condition of the spherical Nb single crystals

  4. Electroerosion impulse effect on W single crystal structure

    International Nuclear Information System (INIS)

    Aleshina, S.A.; Khvostikova, V.D.; Zolotykh, B.N.; Marchuk, A.I.

    1977-01-01

    The mechanism has been studied of brittle failure of single crystal tungsten on planes of crystallographic orientations [100], [110]; [111] in the process of electro-erosion machining by pulses of energies ranging from 1200 to 5000 μJ and of duration of 1 μs. It is shown that the electro-erosion machining of single crystal tungsten is characterized by the formation of a defect layer with a grid of microcracks which lie at a depth of approximately 80 μm. The appearance and the distribution of cracks on the surface of single crystals depends on the crystallogrpahic orientation

  5. Dielectric and baric characteristics of TlS single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Mustafaeva, S.N., E-mail: solmust@gmail.com [Institute of Physics, ANAS, G. Javid prosp. 33, Az 1143 Baku (Azerbaijan); Asadov, M.M. [Institute of Chemical Problems, ANAS, G. Javid prosp. 29, Az 1143 Baku (Azerbaijan); Ismailov, A.A. [Institute of Physics, ANAS, G. Javid prosp. 33, Az 1143 Baku (Azerbaijan)

    2014-11-15

    The investigation of the frequency dependences of the dielectric coefficients and ac-conductivity of the TlS single crystals made it possible to elucidate the nature of dielectric loss and the charge transfer mechanism. Moreover, we evaluated the density and energy spread of localized states near the Fermi level, the average hopping time and the average hopping length. It was shown that the dc-conductivity of the TlS single crystals can be controlled by varying the hydrostatic pressure. This has opened up possibilities for using TlS single crystals as active elements of pressure detectors.

  6. Growth of Ga2O3 single crystal

    OpenAIRE

    龍見, 雅美; 小池, 裕之; 市木, 伸明; Tatsumi, Masami; Koike, Hiroyuki; Ichiki, Nobuaki

    2010-01-01

    Single crystals of β-Ga2O3 for substrates of GaN LED were grown by Floating Zone(FZ) method. The transparent single crystals of 5-6 mm in diameter were reproducibly obtained by applying necking procedure and the preferential growth direction was . Many cracks were induced along the cleavage plane of (100) in slicing process, which is related to thermal stress and the growth direction. However, this preliminary growth experiments suggested that β-Ga2O3 single crystal is promising as a substrat...

  7. Resistivity distribution of silicon single crystals using codoping

    Science.gov (United States)

    Wang, Jong Hoe

    2005-07-01

    Numerous studies including continuous Czochralski method and double crucible technique have been reported on the control of macroscopic axial resistivity distribution in bulk crystal growth. The simple codoping method for improving the productivity of silicon single-crystal growth by controlling axial specific resistivity distribution was proposed by Wang [Jpn. J. Appl. Phys. 43 (2004) 4079]. Wang [J. Crystal Growth 275 (2005) e73] demonstrated using numerical analysis and by experimental results that the axial specific resistivity distribution can be modified in melt growth of silicon crystals and relatively uniform profile is possible by B-P codoping method. In this work, the basic characteristic of 8 in silicon single crystal grown using codoping method is studied and whether proposed method has advantage for the silicon crystal growth is discussed.

  8. Crystallization and diffraction patterns of the oxy and cyano forms of the Lucina pectinata haemoglobins complex

    International Nuclear Information System (INIS)

    Ruiz-Martínez, Carlos R.; Nieves-Marrero, Carlos A.; Estremera-Andújar, Rafael A.; Gavira, José A.; González-Ramírez, Luis A.; López-Garriga, Juan; García-Ruiz, Juan M.

    2008-01-01

    The native oxygen-carrier haemoglobins complex (HbII–III) is composed of haemoglobin II (HbII) and haemoglobin III (HbIII), which are found in the ctenidia tissue of the bivalve mollusc Lucina pectinata. This protein complex was isolated and purified from its natural source and crystallized using the vapour-diffusion and capillary counter-diffusion methods. The native oxygen-carrier haemoglobins complex (HbII–III) is composed of haemoglobin II (HbII) and haemoglobin III (HbIII), which are found in the ctenidia tissue of the bivalve mollusc Lucina pectinata. This protein complex was isolated and purified from its natural source and crystallized using the vapour-diffusion and capillary counter-diffusion methods. Oxy and cyano derivatives of the complex crystallized using several conditions, but the best crystals in terms of quality and size were obtained from sodium formate pH 5 using the counter-diffusion method in a single capillary. Crystals of the oxy and cyano complexes, which showed a ruby-red colour and nonsingular prismatic shapes, scattered X-rays to resolution limits of 2.15 and 2.20 Å, respectively, using a 0.886 Å synchrotron-radiation source. The crystals belonged to the tetragonal system, space group P4 2 2 1 2, with unit-cell parameters a = b = 74.07, c = 152.07 and a = b = 73.83, c = 152.49 Å for the oxy and cyano complexes, respectively. The asymmetric unit of both crystals is composed of a single copy of the heterodimer, with Matthew coefficients (V M ) of 3.08 and 3.06 Å 3 Da −1 for the oxy and cyano complexes, respectively, which correspond to a solvent content of approximately 60.0% by volume

  9. Surface structure modification of single crystal graphite after slow, highly charged ion irradiation

    Science.gov (United States)

    Alzaher, I.; Akcöltekin, S.; Ban-d'Etat, B.; Manil, B.; Dey, K. R.; Been, T.; Boduch, P.; Rothard, H.; Schleberger, M.; Lebius, H.

    2018-04-01

    Single crystal graphite was irradiated by slow, highly charged ions. The modification of the surface structure was studied by means of Low-Energy Electron Diffraction. The observed damage cross section increases with the potential energy, i.e. the charge state of the incident ion, at a constant kinetic energy. The potential energy is more efficient for the damage production than the kinetic energy by more than a factor of twenty. Comparison with earlier results hints to a strong link between early electron creation and later target atom rearrangement. With increasing ion fluence, the initially large-scale single crystal is first transformed into μ m-sized crystals, before complete amorphisation takes place.

  10. Rapid, green synthesis and surface-enhanced Raman scattering effect of single-crystal silver nanocubes

    Science.gov (United States)

    Mao, Aiqin; Jin, Xia; Gu, Xiaolong; Wei, Xiaoqing; Yang, Guojing

    2012-08-01

    Single-crystal silver (Ag) nanocubes have been synthesized by a rapid and green method at room temperature by adding sodium hydroxide solution to the mixed solutions of silver nitrate, glucose and polyvinylpyrrolidone (PVP). The X-ray diffraction (XRD), ultraviolet-visible (UV-visible) and transmission electron microscopy (TEM) were used to characterize the phase composition and morphology. The results showed that the as-prepared particles were single-crystal Ag nanocubes with edge lengths of around 77 nm and a growing direction along {1 0 0} facets. As substrates for surface-enhanced Raman scattering (SERS) experiment on crystal violet (CV), the SERS enhancement factor of the as-prepared Ag nanocubes were measured to be 5.5 × 104, indicating potential applications in chemical and biological analysis.

  11. Study of photoluminescence from annealed bulk-ZnO single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Yoneta, M.; Ohishi, M.; Saito, H. [Department of Applied Physics, Okayama University of Science, 1-1 Ridai-cho, Okayama 700-0005 (Japan); Yoshino, K. [Department of Electrical and Electronic Engineering, Miyazaki University, 1-1 Gakuen Kibanadai-nishi, Miyazaki 889-2192 (Japan); Honda, M. [Faculty of Science, Naruto University of Education, 748 Nakajima, Takashima, Naruto-cho, Naruto-shi 772-8502 (Japan)

    2006-03-15

    We have investigated the influence of rapid thermal annealing on the photoluminescence of bulk-ZnO single crystal. As-grown ZnO wafer, illuminated by 325 nm ultraviolet light at 4.2 K, emitted the visible luminescence of pale green centered of 2.29 eV. The luminescence was observed by the anneal at the temperature range between 400 C and 1000 C, however, its intensity decreased with anneal temperature. The free-exciton and the 2.18 eV emission line were obtained by the anneal at 1200 C for 60 sec. From the X-ray diffraction and the surface morphology measurements, the improvement of the crystallinity of bulk-ZnO crystal were confirmed. We suggest that a rapid thermal annealing technique is convenience to improve the the quality of bul-ZnO single crystals. (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  12. Two convenient low-temperature routes to single crystals of plutonium dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Meredith, Nathan A. [Departments of Chemistry and Biochemistry, University of Notre Dame, Notre Dame, IN 46556 (United States); Wang, Shuao; Diwu, Juan [School of Radiation Medicine and Protection and School of Radiological and Interdisciplinary Sciences, Soochow University, Suzhou, Jiangsu 215123 (China); Albrecht-Schmitt, Thomas E., E-mail: talbrechtschmitt@gmail.com [Department of Chemistry and Biochemistry, Florida State University, Tallahassee, FL 32306 (United States)

    2014-11-15

    Highlights: • Two low-temperature routes to the growth single crystals of plutonium dioxide. • Safer methods of preparing PuO{sub 2} single crystals that do not involve solid-state synthetic techniques. • Solvothermal crystal growth of plutonium dioxide. - Abstract: During the solvothermal synthesis of a low-dimensional borate, KB{sub 5}O{sub 7}(OH){sub 2}⋅2H{sub 2}O, in the presence of Pu(III), single crystals of plutonium dioxide unexpectedly formed. Single crystals of PuO{sub 2} also formed during the hydrothermal synthesis of another borate, Na{sub 2}B{sub 5}O{sub 8}(OH)⋅2H{sub 2}O, in the presence of Pu(III). The reactions were conducted at 170 °C and 150 °C, respectively, which are much lower temperature than previously reported preparations of crystalline PuO{sub 2}. Yellow–green crystals with a tablet habit were characterized by single crystal X-ray diffraction and solid-state UV–vis–NIR absorption spectroscopy. The crystal structure was solved by direct methods with R{sub 1} = 1.26% for 19 unique observed reflections. PuO{sub 2} is cubic, space group Fm3{sup ‾}m, and adopts the fluorite structure type. The lattice parameter was determined to be a = 5.421(5) Å giving a volume of 159.3(2) Å{sup 3}. The absorption spectrum is consistent with Pu(IV)

  13. Exact solution of the Takagi-Taupin equation for dynamical X-ray Bragg diffraction by a crystal with a transition layer

    International Nuclear Information System (INIS)

    Chukhovskii, F.N.; Khapachev, Yu. P.

    1985-01-01

    The general problem of dynamical diffraction on a crystal with a transition layer is theoretically considered. It is shown that the problem of dynamical diffraction on such a crystal can be solved analytically. Special attention is paid to the dependence of the curves of diffractional reflection on the parameters of the transition layer. (author)

  14. Re-examination of the crystal structure of the β-pyrochlore oxide superconductor KOs 2O 6 by X-ray and convergent-beam electron diffraction analyses

    Science.gov (United States)

    Yamaura, Jun-Ichi; Hiroi, Zenji; Tsuda, Kenji; Izawa, Koichi; Ohishi, Yasuo; Tsutsui, Satoshi

    2009-01-01

    The crystal structure of the β-pyrochlore oxide superconductor KOs 2O 6 is re-examined. A single-crystal X-ray diffraction (XRD) analysis at room temperature first revealed that the compound crystallizes in a cubic structure with the centrosymmetric space group Fd3¯m, as in conventional pyrochlore oxides. Later, however, Schuck et al. claimed a different non-centrosymmetric F4¯3m structure based on their single-crystal XRD analysis. To unambiguously determine the true crystal structure of KOs 2O 6, we carried out high-resolution synchrotron powder X-ray and convergent-beam electron diffraction measurements at room temperature. The space group was determined with high reliability to be centrosymmetric Fd3¯m, not F4¯3m. This confirms the importance of the K atom location in a high-symmetry site, which causes unusually large rattling of the K atom.

  15. Sintered pellets: A simple and cost effective method to predict the performance of GGAG:Ce single crystals

    International Nuclear Information System (INIS)

    Meng, Fang; Koschan, Merry; Melcher, Charles L.; Cohen, Peter

    2015-01-01

    Highlights: • Sintered pellets were firstly used to predict the performance of single crystals. • Similar properties between sintered pellets and single crystals were investigated. • B and Ba increase luminescence intensity in pellets and light yield in crystals. • Ca shortens photoluminescence decay in pellets and scintillation decay in crystals. - Abstract: Polycrystalline Gd 3 Ga 3 Al 2 O 12 :Ce (GGAG:Ce) pellets with various codopants were prepared via solid-state synthesis and characterized by X-ray diffraction, radioluminescence (RL), photoluminescence (PL), reflectivity and PL decay measurements. GGAG:Ce pellets codoped with B and Ba were found to have higher RL intensity than pellets with other codopants, while Ca codoping improved the decay time but reduced the RL intensity. These results were strongly correlated with the performance of these codopants in GGAG:Ce single crystals. The light yield of the single crystals codoped with B or Ba was ∼15% higher than the light yield of the GGAG:Ce crystal without codoping, while Ca codoping in single crystals resulted in lower light yield but shorter scintillation decay time (43 ns vs. 56 ns). The consistent performance of these codopants in both matrix forms indicates that sintering pellets may be used as a simple cost effective technique to evaluate compositions for likely single crystal scintillator performance

  16. AIP Single and double diffraction dissociation at the LHC

    CERN Document Server

    Fiore, Roberto; Mieskolainen, Mikael; Orava, Risto

    2017-01-01

    Single and double di ff raction dissociation at the LHC is studied in a factorizable Regge-pole model, dominated by a Pomeron pole exchange in the t channel. While the contribution from secondary reggeon exchanges at the LHC is negligible, they are indispensable to match the lower-energy, ISR and FNAL data. To this end we append to the leading Pomeron exchange an e ff ective reggeon. The main emphasis in our study is on the nucleon resonances in missing masses, that are accounted for by a dual model of the inelastic pP → M X vertex, similar to the DIS structure function, known from HERA, with a non-linear nucleon, N ∗ trajectory in the direct, M 2 X channel. Regge factorization and its breakdown due to a renormalization factor, tempering the energy rise is discussed.

  17. 3.5 W of diffraction-limited green light at 515 nm from SHG of a single-frequency tapered diode laser

    DEFF Research Database (Denmark)

    Jensen, Ole Bjarlin; Hansen, Anders Kragh; Müller, André

    2017-01-01

    Multi-Watt efficient compact green laser sources are required for a number of applications e.g. within biophotonics, laser pumping and laser displays. We present generation of 3.5 W of diffraction-limited green light at 515 nm by second harmonic generation (SHG) of a tapered diode laser, itself...... yielding more than 9 W at 1030 nm. SHG is performed in single pass through a cascade of two nonlinear crystals with re-focusing and dispersion compensating optics between the two nonlinear crystals. The laser is single-frequency and the output power is stabilized to better than ±0.4%....

  18. Growth features of ammonium hydrogen d-tartrate single crystals

    Indian Academy of Sciences (India)

    Unknown

    Abstract. Ammonium hydrogen d-tartrate (d-AHT) single crystals were grown in silica gel. The growth fea- ... solution (specific gravity, 1⋅04 g/cc) with d-tartaric acid solution having ... resulting in the production of crystal nuclei. The interface.

  19. On the growth of calcium tartrate tetrahydrate single crystals

    Indian Academy of Sciences (India)

    Unknown

    Abstract. Calcium tartrate single crystals were grown using silica gel as the growth medium. Calcium for- mate mixed with formic acid was taken as the supernatant solution. It was observed that the nucleation den- sity was reduced and the size of the crystals was improved to a large extent compared to the conventional way.

  20. Crystal growth, spectral and laser properties of Nd:LuAG single crystal

    International Nuclear Information System (INIS)

    Xu, X D; Meng, J Q; Cheng, Y; Li, D Z; Cheng, S S; Wu, F; Zhao, Z W; Wang, X D; Xu, J

    2009-01-01

    Nd:LuAG (Nd:Lu 3 Al 5 O 12 ) crystal was grown by the Czochralski method. X-ray powder diffraction experiments show that the Nd:LuAG crystal crystallizes in the cubic with space group Ia3d and has the cell parameter: a = 1.1907 nm, V = 1.6882 nm 3 . The absorption and fluorescence spectra of Nd:LuAG crystal at room temperature were investigated. With a fiber-coupled diode laser as pump source, the continuous-wave (CW) laser action of Nd:LuAG crystal was demonstrated. The maximum output power at 1064 nm was obtained to be 3.8 W under the incident pump power of 17.3 W, with the optical conversion efficiency 22.0% and the slope efficiency 25.7%