scholarly journals Structural and In Situ X-ray Diffraction Study of Hydrogenation of CaxMg1−xNi2 (0 ≤ x ≤ 1)

Crystals ◽  
2021 ◽  
Vol 12 (1) ◽  
pp. 47
Author(s):  
Zia Ur Rehman ◽  
Mohsan Nawaz ◽  
Hameed Ullah ◽  
Pervaiz Ahmad ◽  
Mayeen Uddin Khandaker ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Powder Diffraction ◽  
Gas Flow ◽  
Hydrogen Gas ◽  
Laves Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Phase Type ◽  
Diffraction Patterns

In the quasi-binary system CaNi2-MgNi2 solid-solutions CaxMg1−xNi2 (0 ≤ x ≤ 1) were prepared from the elements. They crystallize in the hexagonal Laves phase type (MgNi2, C36) for x ≤ 0.33 (P63/mmc, a = 482.51(7) pm, c = 1582.1(3) pm for x = 0, a = 482.59 (3), c = 1583.1(1) for x = 0.33) and in the cubic Laves phase type (MgCu2, C15) for 0.33 < x (Fd−3m, a = 697.12(3) pm for x = 0.5, a = 705.11(2) pm for x = 0.67, a = 724.80(2) pm for x = 1). After hydrogenation in an autoclave the X-ray diffraction patterns changed completely. Reflections assigned to CaNiH3, and Ni and Rietveld refinement confirmed this. The hydrogenation properties of CaxMg1−xNi2 (0 ≤ x ≤ 1) compounds were also studied in situ by X-ray powder diffraction. In situ X-ray powder diffraction of CaxMg1−xNi2 (0 ≤ x ≤ 1) compounds under 0.3 MPa hydrogen gas flow (15 sccm), data collected on a Rigaku SmartLab diffractometer in an Anton Paar XRK 900 Reactor Chamber using Cu-Kα1 radiation. Scanning electron microscopy and EDX spectroscopy confirmed the entitled materials and elemental composition, respectively. From the Transmission electron microscopy and Selected area electron diffraction concluded that the CaxMg1−xNi2 (0 ≤ x ≤ 1) compounds were crystalline.

Development of an in situ synchrotron X-ray total scattering setup under pressurized hydrogen gas

2018 ◽  
Vol 51 (3) ◽  
pp. 796-801 ◽  
Author(s):  
Kouji Sakaki ◽  
Hyunjeong Kim ◽  
Akihiko Machida ◽  
Tetsu Watanuki ◽  
Yoshinori Katayama ◽  
...  
Keyword(s):  
Pair Distribution Function ◽  
Hydrogen Gas ◽  
Ex Situ ◽  
Sample Holder ◽  
Hydrogen Storage Materials ◽  
X Ray Diffraction ◽  
Total Scattering ◽  
X Ray ◽  
Diffraction Patterns

This article describes the development of an in situ gas-loading sample holder for synchrotron X-ray total scattering experiments, particularly for hydrogen storage materials, designed to collect diffraction and pair distribution function (PDF) data under pressurized hydrogen gas. A polyimide capillary with a diameter and thickness of 1.4 and 0.06 mm, respectively, connected with commercially available Swagelok fittings was used as an in situ sample holder. Leakage tests confirmed that this sample holder allows 3 MPa of hydrogen gas pressure and 393 K to be achieved without leakage. Using the developed in situ sample holder, significant background and Bragg peaks from the sample holder were not observed in the X-ray diffraction patterns and their signal-to-noise ratios were sufficiently good. The PDF patterns showed sharp peaks in the r range up to 100 Å. The results of Rietveld and PDF refinements of Ni are consistent with those obtained using a polyimide capillary (1.0 mm diameter and 0.04 mm thickness) that has been used for ex situ experiments. In addition, in situ synchrotron X-ray total scattering experiments under pressurized hydrogen gas up to 1 MPa were successfully demonstrated for LaNi4.6Cu.

Electron Microscopy/Diffraction Study of the Ternary Mn-Er-S System

1990 ◽  
Vol 48 (1) ◽  
pp. 76-77
Author(s):  
A. R. Landa Canovas ◽  
L.C. Otero Diaz ◽  
T. White ◽  
B.G. Hyde
Keyword(s):  
Electron Microscopy ◽  
Gas Flow ◽  
Graphite Crucible ◽  
Nominal Composition ◽  
X Ray Diffraction ◽  
Alumina Crucible ◽  
X Ray ◽  
Intermediate Phases ◽  
Twin Band ◽  
Ar Gas

X-Ray diffraction revealed two intermediate phases in the system MnS+Er2S3,:MnEr2S4= MnS.Er2S3, and MnEr4S7= MnS.2Er2S3. Their structures may be described as NaCl type, chemically twinned at the unit cell level, and isostructural with CaTi2O4, and Y5S7 respectively; i.e. {l13} NaCl twin band widths are (4,4) and (4,3).The present study was to search for structurally-related (twinned B.) structures and or possible disorder, using the more sensitive and appropiate technigue of electron microscopy/diffraction.A sample with nominal composition MnEr2S4 was made by heating Mn3O4 and Er2O3 in a graphite crucible and a 5% H2S in Ar gas flow at 1500°C for 4 hours. A small amount of this material was thenannealed, in an alumina crucible, contained in sealed evacuated silica tube, for 24 days at 1100°C. Both samples were studied by X-ray powder diffraction, and in JEOL 2000 FX and 4000 EX microscopes.

Structural evolution of NASICON-type Li1+xAlxGe2−x(PO4)3 using in situ synchrotron X-ray powder diffraction

2016 ◽  
Vol 4 (20) ◽  
pp. 7718-7726 ◽  
Author(s):  
Dorsasadat Safanama ◽  
Neeraj Sharma ◽  
Rayavarapu Prasada Rao ◽  
Helen E. A. Brand ◽  
Stefan Adams
Keyword(s):  
Solid Electrolyte ◽  
Diffraction Study ◽  
Powder Diffraction ◽  
Structural Evolution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nasicon Type ◽  
Precursor Glass

In situ synchrotron X-ray diffraction study of the synthesis of solid-electrolyte Li1+xAlxGe2−x(PO4)3 (LAGP) from the precursor glass reveals that an initially crystallized dopant poor phase transforms into the Al-doped LAGP at 800 °C.

Late Mesozoic—Cenozoic clay mineral successions of southern Iran and their palaeoclimatic implications

Clay Minerals ◽  
2005 ◽  
Vol 40 (2) ◽  
pp. 191-203 ◽  
Author(s):  
F. Khormali ◽  
A. Abtahi ◽  
H. R. Owliaie
Keyword(s):  
Electron Microscopy ◽  
Upper Cretaceous ◽  
Sedimentary Rocks ◽  
X Ray Diffraction ◽  
Humid Climate ◽  
X Ray ◽  
Late Mesozoic ◽  
Southern Iran ◽  
Transmission Electron

AbstractClay minerals of calcareous sedimentary rocks of southern Iran, part of the old Tethys area, were investigated in order to determine their origin and distribution, and to reconstruct the palaeoclimate of the area. Chemical analysis, X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and thin-section studies were performed on the 16 major sedimentary rocks of the Fars and Kuhgiluyeh Boyerahmad Provinces.Kaolinite, smectite, chlorite, illite, palygorskite and illite-smectite interstratified minerals were detected in the rocks studied. The results revealed that detrital input is possibly the main source of kaolinite, smectite, chlorite and illite, whilein situneoformation during the Tertiary shallow saline and alkaline environment could be the dominant cause of palygorskite occurrences in the sedimentary rocks.The presence of a large amount of kaolinite in the Lower Cretaceous sediments and the absence or rare occurrence of chlorite, smectite, palygorskite and illite are in accordance with the warm and humid climate of that period. Smaller amounts of kaolinite and the occurrence of smectite in Upper Cretaceous sediments indicate the gradual shift from warm and humid to more seasonal climate. The occurrence of palygorskite and smectite and the disappearance of kaolinite in the late Palaeocene sediments indicate the increase in aridity which has probably continued to the present time.

Applications of High-Resolution Powder X-Ray Diffraction

2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch
Keyword(s):  
High Resolution ◽  
Synchrotron Radiation ◽  
Powder Diffraction ◽  
X Rays ◽  
X Ray Diffraction ◽  
Crystalline Materials ◽  
X Ray ◽  
Structural Characterisation ◽  
Pdf Analysis

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.

Size dependent behavior of Fe3O4crystals during electrochemical (de)lithiation: an in situ X-ray diffraction, ex situ X-ray absorption spectroscopy, transmission electron microscopy and theoretical investigation

2017 ◽  
Vol 19 (31) ◽  
pp. 20867-20880 ◽  
Author(s):  
David C. Bock ◽  
Christopher J. Pelliccione ◽  
Wei Zhang ◽  
Janis Timoshenko ◽  
K. W. Knehr ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Structural Changes ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
X Ray ◽  
Size Dependent ◽  
Transmission Electron ◽  
Dependent Behavior ◽  
X Ray Absorption

Crystal and atomic structural changes of Fe3O4upon electrochemical (de)lithiation were determined.

scholarly journals Green bio-inspired synthesis, characterization and activity of silver nanoparticle forms of Centaurea virgata Lam. and the isolated flavonoid eupatorin

2018 ◽  
Vol 7 (4) ◽  
pp. 372-379 ◽  
Author(s):  
Burcu Sümer Tüzün ◽  
Judit Hohmann ◽  
Bijen Kivcak
Keyword(s):  
Electron Microscopy ◽  
Zeta Potential ◽  
Synthesis Method ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Characteristic Absorption Band ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Diffraction Patterns ◽  
Isolated Compound

AbstractA green synthesis method of silver nanoparticles (AgNPs) usingCentaurea virgataLam. extract and the isolated compound eupatorin was investigated in this study. Ultraviolet-visible (UV-Vis) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM)/energy-dispersive X-ray (EDX) spectroscopy, thermal gravimetric analysis, X-ray diffraction analysis and zeta potential were used for characterization of AgNPs. The UV-Vis spectrum exhibited a characteristic absorption band at 420 nm for monodisperse nanoparticles. FTIR measurements also proved the formation. X-ray diffraction patterns showed peaks at (110) and (112), which are characteristic for hexagonal crystals and also showed peaks at (111), (200) and (240), which are characteristic for orthorhombic crystals. The TEM images of AgNPs show that the morphology of AgNPs was predominantly spherical. Obtained AgNPs were highly stable according to the zeta potential values. The nitric oxide scavenging activity, which is also related to anticancer activity, of AgNPs was evaluated. It can be concluded thatC. virgataLam. extract and eupatorin can be used as a reducing agent for potential antioxidant AgNP formation.

In-Situ Diffraction Studies of Gas Storage Materials on a Laboratory X-Ray System

2013 ◽  
Vol 1544 ◽  
Author(s):  
Marco Sommariva ◽  
Harald van Weeren ◽  
Olga Narygina ◽  
Jan-André Gertenbach ◽  
Christian Resch ◽  
...  
Keyword(s):  
Large Scale ◽  
Fossil Fuels ◽  
Reaction Chamber ◽  
Hydrogen Gas ◽  
Gas Pressure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structural Modifications ◽  
Model Studies

ABSTRACTThe sorption processes for hydrogen and carbon dioxide are of considerable, and growing interest, particularly due to their relevance to a society that seeks to replace fossil fuels with a more sustainable energy source. X-ray diffraction allows a unique perspective for studying structural modifications and reaction mechanisms that occur when gas and solid interact. The fundamental challenge associated with such a study is that experiments are conducted while the solid sample is held under a gas pressure. To date in-situ high gas pressure studies of this nature have typically been undertaken at large-scale facilities such as synchrotrons or on dedicated laboratory instruments. Here we report high-pressure XRD studies carried out on a multi-purpose diffractometer. To demonstrate the suitability of the equipment, two model studies were carried out, firstly the reversible hydrogen cycling over LaNi5, and secondly the structural change that occurs during the decomposition of ammonia borane that results in the generation of hydrogen gas in the reaction chamber. The results have been finally compared to the literature. The study has been made possible by the combination of rapid X-ray detectors with a reaction chamber capable of withstanding gas pressures up to 100 bar and temperatures up to 900 °C.

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