In situhydrogen loading on zirconium powder

For the first time, various hydride phases in a zirconium–hydrogen system have been prepared in a high-energy synchrotron X-ray radiation beamline and their transformation behaviour has been studiedin situ. First, the formation and dissolution of hydrides in commercially pure zirconium powder were monitored in real time during hydrogenation and dehydrogenation, then whole pattern crystal structure analysis such as Rietveld and Pawley refinements were performed. All commonly reported low-pressure phases presented in the Zr–H phase diagram are obtained from a single experimental arrangement.

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Raman Spectroscopy and Single-Crystal High-Temperature Investigations of Bentorite, Ca6Cr2(SO4)3(OH)12·26H2O

Minerals ◽

10.3390/min10010038 ◽

2019 ◽

Vol 10 (1) ◽

pp. 38

Author(s):

Rafał Juroszek ◽

Biljana Krüger ◽

Irina Galuskina ◽

Hannes Krüger ◽

Martina Tribus ◽

...

Keyword(s):

Crystal Structure ◽

High Temperature ◽

Single Crystal ◽

Chemical Formula ◽

Crystal Chemical Formula ◽

Single Crystal Diffraction ◽

Bending Vibrations ◽

X Ray ◽

First Time

The crystal structure of bentorite, ideally Ca6Cr2(SO4)3(OH)12·26H2O, a Cr3+ analogue of ettringite, is for the first time investigated using X-ray single crystal diffraction. Bentorite crystals of suitable quality were found in the Arad Stone Quarry within the pyrometamorphic rock of the Hatrurim Complex (Mottled Zone). The preliminary semi-quantitative data on the bentorite composition obtained by SEM-EDS show that the average Cr/(Cr + Al) ratio of this sample is >0.8. Bentorite crystallizes in space group P31c, with a = b = 11.1927(5) Å, c =21.7121(10) Å, V = 2355.60(18) Å3, and Z = 2. The crystal structure is refined, including the hydrogen atom positions, to an agreement index R1 = 3.88%. The bentorite crystal chemical formula is Ca6(Cr1.613Al0.387)Σ2[(SO4)2.750(CO3)0.499]Σ3.249(OH)11.502·~25.75H2O. The Raman spectra of bentorite from two different localities exhibit the presence of the main stretching and bending vibrations related to the sulfate group at 983 cm−1 (ν1), 1109 cm−1 (ν3), 442 cm−1 (ν2), and 601 cm−1 (ν4). Moreover, the presence of bands assigned to the symmetric Cr(OH)63− stretching mode and hydroxyl deformation vibrations of Cr–OH units at ~540 cm−1 and ~757 cm−1, respectively, may be used to distinguish between ettringite and bentorite. In situ high temperature single crystal XRD experiments show that the decomposition of bentorite starts at ca. 45 °C and that a dehydroxylation product similar to metaettringite is formed.

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Synthetic Access to a Novel Binaphthyl Ligand Bearing a Phosphine and a Triazole Donor Site

Zeitschrift für Naturforschung B ◽

10.1515/znb-2009-11-1226 ◽

2009 ◽

Vol 64 (11-12) ◽

pp. 1438-1448 ◽

Cited By ~ 5

Author(s):

Claudia May ◽

Yu Sun ◽

Gotthelf Wolmershäuser ◽

Werner R. Thiel

Keyword(s):

Crystal Structure ◽

Coordination Chemistry ◽

Structure Analysis ◽

Donor Site ◽

Crystal Structure Analysis ◽

Pure Compound ◽

Enantiomerically Pure ◽

X Ray ◽

First Time

The combination of a diphenylphospinyl and a triazol-3-yl unit was realized for the first time at a 1,1'-binaphthyl backbone. This novel type of P,N-ligand is accessible as an enantiomerically pure compound in just a few steps. First experiments on the coordination chemistry with palladium(II) chloride have been carried out. A series of intermediates and a binuclear palladium(II) complex could be characterized by X-ray crystal structure analysis

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Crystal Structure Analysis of a Hexatungstate by a High-Energy X-ray Diffraction Experiment Using an Imaging Plate Weissenberg Camera at the BL04B2 Beamline of SPring-8

Chemistry Letters ◽

10.1246/cl.2001.804 ◽

2001 ◽

Vol 30 (8) ◽

pp. 804-805 ◽

Cited By ~ 13

Author(s):

Tomoji Ozeki ◽

Katsuhiro Kusaka ◽

Noritaka Honma ◽

Yuji Nakamura ◽

Setsuko Nakamura ◽

...

Keyword(s):

Crystal Structure ◽

Structure Analysis ◽

High Energy ◽

Crystal Structure Analysis ◽

Imaging Plate ◽

Diffraction Experiment ◽

X Ray Diffraction ◽

X Ray

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Crystal structure of magnesium dichloride decahydrate determined by X-ray and neutron diffraction under high pressure

Acta Crystallographica Section B Structural Science Crystal Engineering and Materials ◽

10.1107/s205252061500027x ◽

2015 ◽

Vol 71 (1) ◽

pp. 74-80 ◽

Cited By ~ 11

Author(s):

Kazuki Komatsu ◽

Ayako Shinozaki ◽

Shinichi Machida ◽

Takuto Matsubayashi ◽

Mao Watanabe ◽

...

Keyword(s):

Crystal Structure ◽

Neutron Diffraction ◽

Amorphous State ◽

Water Molecules ◽

X Ray ◽

The Difference ◽

Diffraction Patterns ◽

Difference Fourier ◽

First Time

Magnesium dichloride decahydrate (MgCl2·10H2O) and its deuterated counterpart (MgCl2·10D2O) are identified for the first time byin-situpowder synchrotron X-ray and spallation neutron diffraction. These substances are crystallized from a previously unidentified nanocrystalline compound, which originates from an amorphous state at low temperature. A combination of a recently developed autoindexing procedure and the charge-flipping method reveals that the crystal structure of MgCl2·10H2O consists of an ABCABC... sequence of Mg(H2O)6octahedra. The Cl−anions and remaining water molecules unconnected to the Mg2+cations bind the octahedra, similar to other water-rich magnesium dichloride hydrates. The D positions in MgCl2·10D2O, determined by the difference Fourier methods using the neutron powder diffraction patterns at 2.5 GPa, show the features such as bifurcated hydrogen bonds and tetrahedrally coordinated O atoms, which were not found in other forms of magnesium chloride hydrates.

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A New Synthetic Route to (Trifluoromethyl)quinolines: Nickel-Catalyzed Insertion of an Alkyne into an Aromatic C–S Bond by Formation of a Thianickelacycle and Thermal Desulfidation

Synlett ◽

10.1055/s-0037-1610785 ◽

2021 ◽

Author(s):

Takuya Kurahashi ◽

Seijiro Matsubara ◽

Tasuku Inami

Keyword(s):

Crystal Structure ◽

Fine Structure ◽

Sulfur Atom ◽

Crystal Structure Analysis ◽

Insertion Reaction ◽

Synthetic Route ◽

X Ray ◽

X Ray Absorption ◽

Single Crystal Structure Analysis

AbstractWe have developed a nickel-catalyzed insertion reaction of an alkyne into a 2-(trifluoromethyl)-1,3-benzothiazole to give a seven-membered benzothiazepine that is converted into a 2-(trifluoromethyl)quinoline by thermal desulfidation. This process can be considered a formal substitution of a sulfur atom with an alkyne. The structure of the thianickelacycle intermediate formed through oxidative addition of a C–S bond in the benzothiazole to nickel(0) was confirmed by X-ray single-crystal structure analysis and in situ X-ray absorption fine-structure spectroscopy.

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Structural evolution of high energy density V3+/V4+ mixed valent Na3V2O2x(PO4)2F3−2x (x = 0.8) sodium vanadium fluorophosphate using in situ synchrotron X-ray powder diffraction

Journal of Materials Chemistry A ◽

10.1039/c4ta00773e ◽

2014 ◽

Vol 2 (21) ◽

pp. 7766-7779 ◽

Cited By ~ 43

Author(s):

Paula Serras ◽

Verónica Palomares ◽

Teófilo Rojo ◽

Helen E. A. Brand ◽

Neeraj Sharma

Keyword(s):

Structural Evolution ◽

High Energy ◽

High Energy Density ◽

Sodium Ion Battery ◽

Time Resolved ◽

X Ray ◽

Xrd Study ◽

First Time ◽

Synchrotron Xrd

The first time-resolved in situ synchrotron XRD study of a cathode in a functioning sodium-ion battery. We determine the reaction mechanism, lattice parameters, sodium evolution, and the maximum sodium extraction for the fresh and precycled cell.

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In-Situ Rheed-Traxs Monitoring Alloy Composition of the Surface During RF-MBE Growth of GaInN and AIGaN

MRS Proceedings ◽

10.1557/proc-482-441 ◽

1997 ◽

Vol 482 ◽

Author(s):

A. Ito ◽

H. Sakai ◽

M. Inagaki ◽

G. Nomura ◽

Y Nakamura ◽

...

Keyword(s):

Alloy Composition ◽

High Energy ◽

Alloy Layer ◽

Solid Alloy ◽

High Energy Electron ◽

Mbe Growth ◽

X Ray ◽

Reflection Angle ◽

First Time

AbstractIn-situ reflection high energy electron diffraction total reflection angle X-ray spectroscopy (RHEED-TRAXS) was performed to monitor alloy composition at the surface during growth of nitrides by RF-MBE for the first time. TRAXS signal of the GaLα line is found to be more sensitive to the composition at the surface than the GaKαline. A difference in the composition of layer adsorbed on the surface and the solid alloy layer has been identified.

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Investigation of reaction conditions on synthesis of steroidal bromohydrin and structural analysis of novel 6α-brom-5β-hydroxy derivative

Facta universitatis - series Physics Chemistry and Technology ◽

10.2298/fupct1802219k ◽

2018 ◽

Vol 16 (2) ◽

pp. 219-228

Author(s):

Ivana Kuzminac ◽

Olivera Klisuric ◽

Andrea Nikolic ◽

Marija Sakac

Keyword(s):

Crystal Structure ◽

Perchloric Acid ◽

Crystal Structure Analysis ◽

Hydroxy Derivative ◽

Reaction Products ◽

Reaction Conditions ◽

X Ray ◽

Hypobromous Acid ◽

Series Of Experiments

Reaction conditions variation and its influence on the reaction of 3?- acetoxy-17-oxa-17a-homoandrost-5-en-16-one with in situ generated hypobromous acid was investigated. Hypobromous acid was generated from N-bromoacetamide or Nbromosuccinimide and perchloric acid, and as solvent dioxane, dimethoxyethane or tetrahydrofuran were used. After a series of experiments, it was determined that the number of the reaction products depends on the reagent used, solvents, perchloric acid concentration and the presence/absence of daylight. It has also been found that the yields of certain compounds depend also on the reaction time and temperature. 6?-Bromo-5?- hydroxy derivate is obtained by usage of NBA and 0.28 M perchloric acid in dioxane on daylight. Its structure was confirmed by NMR and X-ray crystal structure analysis.

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Epitaxial Film Growth of Single Crystal Ce/V Prepared by Molecular-Beam Epitaxy

MRS Proceedings ◽

10.1557/proc-77-557 ◽

1986 ◽

Vol 77 ◽

Author(s):

Hitoshi Homma ◽

Kai-Y. Yang ◽

Ivan K. Schuller

Keyword(s):

Single Crystal ◽

Film Growth ◽

High Energy ◽

Epitaxial Films ◽

X Ray ◽

X Ray Scattering ◽

Crystal Film ◽

Epitaxial Film Growth ◽

First Time

ABSTRACTThe growth of epitaxial films of cerium (Ce)/vanadium (V)/on single crystal sapphires (α-A1203) was studied by in-situ reflection high energy electron diffraction and x-ray scattering. For the first time Ce(111) single crystal film was grown on V(110)/α-A12O3 (1120) in the Frank-van der Merwe mode. A new epitaxial orientation, different from the well known Nishiyama-Wasserman or Kurdjumov-Sachs orientations is found in the present study. Subsequent V(110) layers grow epitaxially with three equivalent domains.

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