scholarly journals Fast continuous measurement of synchrotron powder diffraction synchronized with controlling gas and vapour pressures at beamline BL02B2 of SPring-8

2020 ◽  
Vol 27 (3) ◽  
pp. 616-624 ◽  
Author(s):  
Shogo Kawaguchi ◽  
Michitaka Takemoto ◽  
Hideki Tanaka ◽  
Shotaro Hiraide ◽  
Kunihisa Sugimoto ◽  
...  
Keyword(s):  
Control System ◽  
High Resolution ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Pressure Control ◽  
Diffraction Measurement ◽  
Line System ◽  
Synchrotron Powder Diffraction ◽  
Pressure Control System

A gas- and vapour-pressure control system synchronized with the continuous data acquisition of millisecond high-resolution powder diffraction measurements was developed to study structural change processes in gas storage and reaction materials such as metal organic framework compounds, zeolite and layered double hydroxide. The apparatus, which can be set up on beamline BL02B2 at SPring-8, mainly comprises a pressure control system of gases and vapour, a gas cell for a capillary sample, and six one-dimensional solid-state (MYTHEN) detectors. The pressure control system can be remotely controlled via developed software connected to a diffraction measurement system and can be operated in the closed gas and vapour line system. By using the temperature-control system on the sample, high-resolution powder diffraction data can be obtained under gas and vapour pressures ranging from 1 Pa to 130 kPa in temperatures ranging from 30 to 1473 K. This system enables one to perform automatic and high-throughput in situ X-ray powder diffraction experiments even at extremely low pressures. Furthermore, this developed system is useful for studying crystal structures during the adsorption/desorption processes, as acquired by millisecond and continuous powder diffraction measurements. The acquisition of diffraction data can be synchronized with the control of the pressure with a high frame rate of up to 100 Hz. In situ and time-resolved powder diffraction measurements are demonstrated for nanoporous Cu coordination polymer in various gas and vapour atmospheres.

Structure of a new high-pressure–high-temperature modification of antimony(III) oxide, γ-Sb2O3, from high-resolution synchrotron powder diffraction data

2012 ◽  
Vol 68 (1) ◽  
pp. 1-7 ◽  
Author(s):  
Denis Orosel ◽  
Robert E. Dinnebier ◽  
Vladislav A. Blatov ◽  
Martin Jansen
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
High Resolution ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Powder Diffraction Data ◽  
Temperature Modification ◽  
Synchrotron Powder Diffraction ◽  
High Pressure High Temperature ◽  
High Temperature Modification

A quenchable new high-pressure–high-temperature modification of antimony(III) oxide, γ-Sb2O3, has been obtained at hydrostatic pressures of 9–11 GPa and temperatures of 573–773 K. Its crystal structure has been determined from high-resolution synchrotron powder diffraction data. γ-Sb2O3 consists of three-dimensionally cross-linked infinite chains of SbO3 E units (E = lone pair) with the chains forming tetragonal rod-packing. The underlying topology of γ-Sb2O3 (3,3T8) is found very rarely in inorganic structures; it is realised only for the polyanion [Si4O4N6]10− that occurs in the Ce4(Si4O4N6)O structure type. The structural relation to the two previously known polymorphs of Sb2O3 at ambient pressure, valentinite and senarmontite is discussed.

Structures of three dehydration products of bischofite from in situ synchrotron powder diffraction data (MgCl2·nH2O; n = 1, 2, 4)

2007 ◽  
Vol 63 (2) ◽  
pp. 235-242 ◽  
Author(s):  
Kunihisa Sugimoto ◽  
Robert E. Dinnebier ◽  
Jonathan C. Hanson
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Similarity Criteria ◽  
Powder Diffraction Data ◽  
Rietveld Refinements ◽  
Synchrotron Powder Diffraction ◽  
Magnesia Concrete ◽  
First Time

High-quality in situ synchrotron powder diffraction data have been used to investigate the decomposition products of bischofite in the temperature range 298 ≤ T ≤ 873 K. At least eight phases could be identified: MgCl2·nH2O (n = 1, 2, 4 and 6), MgOHCl·nH2O (0 ≤ n ≤ 1.0), MgCl2 and MgO. The crystal structures of three magnesium chloride hydrates MgCl2·nH2O (n = 1, 2, 4) were determined ab initio, replacing published Rietveld refinements from low-quality powder diffraction data based on similarity criteria. MgCl2·4H2O was found to be disordered and has been correctly determined for the first time. The crystal structures of bischofite and MgCl2·4H2O consist of discrete Mg(H2O)6 and MgCl2(H2O)4 octahedra, respectively. The crystal structure of MgCl2·2H2O is formed by single chains of edge-sharing MgCl2(H2O)4 octahedra, while in the case of MgCl2·H2O double chains of edge-sharing MgCl(H2O)5 octahedra are found. The phases in the system MgCl2–H2O are intermediates in the technologically important process of MgO and subsequently Mg production. The same phases were recently found to be of key importance in the understanding of cracks in certain magnesia concrete floors.

Crystal structure of the inclusion complex of β-cyclodextrin with mefenamic acid from high-resolution synchrotron powder-diffraction data in combination with molecular-mechanics calculations

2002 ◽  
Vol 58 (6) ◽  
pp. 1036-1043 ◽  
Author(s):  
Mihaela M. Pop ◽  
Kees Goubitz ◽  
Gheorghe Borodi ◽  
Mircea Bogdan ◽  
Dirk J. A. De Ridder ◽  
...  
Keyword(s):  
Crystal Structure ◽  
High Resolution ◽  
Inclusion Complex ◽  
Molecular Mechanics ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Mefenamic Acid ◽  
Powder Diffraction Data ◽  
Molecular Mechanics Calculations ◽  
Synchrotron Powder Diffraction

The crystal structure of the inclusion complex of β-cyclo-dextrin with mefenamic acid has been determined from a combination of high-resolution synchrotron powder-diffraction data and molecular-mechanics calculations. A grid search indicates two possible solutions, which are corroborated by molecular-mechanics calculations, while Rietveld-refinement results suggest the crystal structure that is more likely to be formed in the solid state. Mefenamic acid is partially included in β-cyclodextrin with either the xylyl or the benzoic-acid moiety being inside its cavity. In both solutions mefenamic acid and β-cyclodextrin form a monomeric complex in a herringbone packing scheme.

Structure determination of two metal-organic complexes from high-resolution synchrotron powder diffraction data

2001 ◽  
Vol 8 (6) ◽  
pp. 1186-1190 ◽  
Author(s):  
Eva Dova ◽  
Kees Goubitz ◽  
Arjen van Langevelde ◽  
René Driessen ◽  
Taasje Mahabiersing ◽  
...  
Keyword(s):  
High Resolution ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Structure Determination ◽  
Powder Diffraction Data ◽  
Organic Complexes ◽  
Synchrotron Powder Diffraction ◽  
Metal Organic

Crystal Structure of Melaminium Orthophosphate from High-Resolution Synchrotron Powder-Diffraction Data

2004 ◽  
Vol 87 (7) ◽  
pp. 1894-1905 ◽  
Author(s):  
Dirk J. A. De Ridder ◽  
Kees Goubitz ◽  
Vladimir Brodski ◽  
René Peschar ◽  
Henk Schenk
Keyword(s):  
Crystal Structure ◽  
High Resolution ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Powder Diffraction Data ◽  
Synchrotron Powder Diffraction

Cs2Zn(CN)4: a first example of a non-cyano spinel of composition A2M(CN)4 with A=alkali metal and M=group 12 metal

2020 ◽  
Vol 75 (1-2) ◽  
pp. 97-103
Author(s):  
Melanie Werker ◽  
Uwe Ruschewitz
Keyword(s):  
Crystal Structure ◽  
Phase Transition ◽  
High Resolution ◽  
Alkali Metal ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Powder Diffraction Data ◽  
Synchrotron Powder Diffraction ◽  
Group 12 ◽  
Reversible Melting

AbstractThe crystal structure of monoclinic Cs2Zn(CN)4 (C2/c, Z = 4) was solved and refined from high-resolution synchrotron powder diffraction data (ESRF: Swiss-Norwegian beamline). In contrast to all other known cyanides of composition A2M(CN)4 with A = alkali metal and M = group 12 metal, which crystallize in cubic or rhombohedrally distorted spinel variants and thus with A+ in an octahedral coordination, the Cs+ cation in Cs2Zn(CN)4 shows an eight-fold coordination by CN− anions of the [Zn(CN)4]2− tetrahedra. Upon heating, no phase transition is observed. Instead, a reversible melting at approx. T = 380°C occurs.

Sign in / Sign up

Export Citation Format

Share Document