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.

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.

scholarly journals Exploring the origins of crystallisation kinetics in hierarchical materials using in situ X-ray diffraction and pair distribution function analysis

2020 ◽  
Vol 22 (34) ◽  
pp. 18860-18867 ◽  
Author(s):  
Matthew E. Potter ◽  
Mark E. Light ◽  
Daniel J. M. Irving ◽  
Alice E. Oakley ◽  
Stephanie Chapman ◽  
...  
Keyword(s):  
Distribution Function ◽  
Pair Distribution Function ◽  
Function Analysis ◽  
X Ray Diffraction ◽  
Crystallisation Kinetics ◽  
Total Scattering ◽  
Hierarchically Porous ◽  
X Ray ◽  
Scattering Measurements

Novel in situ synchrotron total scattering measurements probe the assembly of primary building units into templated hierarchically porous aluminophosphate catalysts, providing unique insights to understanding crystallisation kinetics.

Structural Studies of Hydrogen Storage Alloys using X-ray/Neutron Diffraction and Total Scattering

2011 ◽  
Vol 1334 ◽  
Author(s):  
Yumiko Nakamura ◽  
Hyunjeong Kim ◽  
Saishun Yamazaki ◽  
Kouji Sakaki ◽  
Thomas Proffen ◽  
...  
Keyword(s):  
Neutron Diffraction ◽  
Pair Distribution Function ◽  
Ex Situ ◽  
Structural Studies ◽  
Hydrogen Storage Alloys ◽  
Total Scattering ◽  
X Ray ◽  
Local Structures ◽  
Rich Domain

ABSTRACTCrystal and local structures and hydrogen occupation of Mg containing materials, (Mg,Ca)Nix (x = 2, 3) intermetallic compounds and a MgCo metastable alloy, have been investigated using in-situ and ex-situ X-ray/neutron diffraction and total scattering.A C15 Laves phase (Mg0.67Ca0.33)Ni2 showed isotropic lattice expansion upon hydrogenation. Mg and Ca occupied the same site randomly. It has two hydrogen sites, Mg(Ca)2Ni2 site and M(Ca)Ni3 site.Mg2CaNi9, MgCa2Ni9, and CaNi3 compounds consisted of MgZn2-type (Mg,Ca)2Ni4 cell and CaCu5-type CaNi5 cell stacking along the c-axis. The MgZn2-type cell was occupied by only Mg in Mg2CaNi9, and randomly occupied by both Mg and Ca in MgCa2Ni9. Expansion of this cell strongly depended on the composition: larger expansion was observed in a Ca-rich composition.Local structure of a Mg-Co alloy synthesized by mechanical alloying has been studied using the PDF (Pair Distribution Function) method. The analysis suggested that material contained two 1-2 nm domains with different compositions and local structures, i.e. Mg-rich and Co-rich domains, and hydrogen was located only in the Mg-rich domain.

scholarly journals In-situ hydrogen gas loading setup for synchrotron X-ray total scattering

2014 ◽  
Vol 70 (a1) ◽  
pp. C868-C868
Author(s):  
Hyunjeong Kim ◽  
Kouji Sakaki ◽  
Kohta Asano ◽  
Miho Yamauchi ◽  
Akihiko Machida ◽  
...  
Keyword(s):  
Hydrogen Storage ◽  
Structural Features ◽  
Hydrogen Gas ◽  
Hydrogen Storage Materials ◽  
Energy Agency ◽  
Promising Alternative ◽  
Total Scattering ◽  
X Ray ◽  
Storage Materials

Hydrogen has been considered as a promising alternative fuel for transportation, provided we can find a way to store a large amount of hydrogen in a compact way. The realization of such a storage system can be achieved by developing materials that can easily absorb, safely store, and rapidly release hydrogen repeatedly. However, there is currently no material to meet all the requirements for on board storage. Great efforts have been made to understand hydrogenation properties of currently available materials to look for a way to improve properties or to prepare new materials. However, investigating the structure of some of these materials is challenging since their hydrides are only available under hydrogen gas pressure. Furthermore, many novel materials with improved properties often show heavily disordered or nanoscale structural features which are difficult to characterize using conventional crystallographic technique alone (crystallographically challenged hydrogen storage materials). In order to investigate the structural change in crystallographically challenged hydrogen storage materials during hydrogenation or dehydrogenation processes we have developed in-situ hydrogen gas loading setup for synchrotron X-ray total scattering experiments at the Japan Atomic Energy Agency (JAEA) beamline of BL22XU [1] at SPring-8. Coupled to an area detector [1,2], this setup allows us to obtain the atomic pair distribution function (PDF) [3] of metal hydrides either in equilibrium or in non-equilibrium state with hydrogen. In this poster, we will introduce our in-situ setup and present some preliminary results on AB5-type intermetallic compounds and Pd nanoparticles.

In Situ X-Ray Diffraction Investigations during Diffusion Anneals of Ni-Cu Thin Film Diffusion Couples

2010 ◽  
Vol 89-91 ◽  
pp. 503-508 ◽  
Author(s):  
J. Sheng ◽  
U. Welzel ◽  
Eric J. Mittemeijer
Keyword(s):  
Thermal Stresses ◽  
Stress Generation ◽  
Ex Situ ◽  
Diffusion Annealing ◽  
X Ray Diffraction ◽  
Individual Layer ◽  
X Ray ◽  
Bilayer System ◽  
Stress Changes

The stress evolution during diffusion annealing of Ni-Cu bilayers (individual layer thicknesses of 50 nm) was investigated employing ex-situ and in-situ X-ray diffraction measurements. Annealing at relatively low homologous temperatures (about 0.3 - 0.4 Tm) for durations up to about 100 hours results in considerable diffusional intermixing, as demonstrated by Auger-electron spectroscopy investigations (in combination with sputter-depth profiling). In addition to thermal stresses due to differences of the coefficients of thermal expansion of layers and substrate, tensile stress con-tributions in the sublayers arise during the diffusion anneals. The obtained stress data have been discussed in terms of possible mechanisms of stress generation. The influence of diffusion on stress development in the sublayers of the diffusion couple during heating and isothermal annealing was investigated by comparing stress changes in the bilayer system with corresponding results obtained under identical conditions for single layers of the components in the bilayer system. The specific residual stresses that emerge due to diffusion between the (sub)layers in the bilayer could thereby be identified.

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 A study on preparation and characterization of carbon doped TiO2 nanotubes

2014 ◽  
Vol 6 (1) ◽  
Author(s):  
Srimala Sreekantan ◽  
Roshasnorlyza Hazan ◽  
Zainovia Lockman ◽  
Ishak Mat
Keyword(s):  
Methyl Orange ◽  
Tio2 Nanotubes ◽  
Pure Tio2 ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
Methyl Orange Degradation ◽  
Doped Tio2 ◽  
X Ray ◽  
Carbon Doped

The present study is directed to clarify the influence of carbon doping on the degradation of methyl orange. TiO2 nanotubes were prepared by anodizing titanium foils in a two electrode configuration bath with titanium foil as the anode and platinum as the counter electrode. The electrochemical bathconsists of 1 M Na2SO4 with 0.7 g ammonium fluoride, NH4F. The nanotubes obtained were further doped with carbon via in-situ and ex-situ method. Incorporation of carbon on TiO2 via in-situ method is accomplished during the anodization process by introducing oxalic acid into electrolyte while theex-situ doping involves carbon incorporation into pre-fabricated TiO2 nanotube via flame annealing using carbon blackN330. Characterization such as Scanning Electron Microscope (SEM), Energy Dispersive X-ray Analysis (EDX), and X-Ray Diffraction (XRD) are used to determine the surfacemorphology, composition of dopants, and phases exists. Well ordered nanotube with good adherence and smooth surface was obtained for both methods. When the oxide was annealed, X-ray diffraction analysis revealed the presence of anatase and rutile phase. The photocatalytic properties of thepure TiO2 and carbon doped TiO2 were tested for methyl orange degradation and the result indicated that the in-situ doped TiO2 has much better degradation than the ex-situ and pure TiO2. The percentage of methyl orange degradation for in-situ was 20% and 41% higher than ex-situ doped TiO2 and pure TiO2, respectively.

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.

scholarly journals The Viscosity and Atomic Structure of Volatile-Bearing Melilititic Melts at High Pressure and Temperature and the Transport of Deep Carbon

Minerals ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 267 ◽  
Author(s):  
Vincenzo Stagno ◽  
Veronica Stopponi ◽  
Yoshio Kono ◽  
Annalisa D’Arco ◽  
Stefano Lupi ◽  
...  
Keyword(s):  
Experimental Data ◽  
High Pressure ◽  
Atomic Structure ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
High Pressure And Temperature ◽  
X Ray ◽  
Falling Sphere ◽  
Basaltic Melts

Understanding the viscosity of mantle-derived magmas is needed to model their migration mechanisms and ascent rate from the source rock to the surface. High pressure–temperature experimental data are now available on the viscosity of synthetic melts, pure carbonatitic to carbonate–silicate compositions, anhydrous basalts, dacites and rhyolites. However, the viscosity of volatile-bearing melilititic melts, among the most plausible carriers of deep carbon, has not been investigated. In this study, we experimentally determined the viscosity of synthetic liquids with ~31 and ~39 wt% SiO2, 1.60 and 1.42 wt% CO2 and 5.7 and 1 wt% H2O, respectively, at pressures from 1 to 4.7 GPa and temperatures between 1265 and 1755 °C, using the falling-sphere technique combined with in situ X-ray radiography. Our results show viscosities between 0.1044 and 2.1221 Pa·s, with a clear dependence on temperature and SiO2 content. The atomic structure of both melt compositions was also determined at high pressure and temperature, using in situ multi-angle energy-dispersive X-ray diffraction supported by ex situ microFTIR and microRaman spectroscopic measurements. Our results yield evidence that the T–T and T–O (T = Si,Al) interatomic distances of ultrabasic melts are higher than those for basaltic melts known from similar recent studies. Based on our experimental data, melilititic melts are expected to migrate at a rate ~from 2 to 57 km·yr−1 in the present-day or the Archaean mantle, respectively.

In situ coupling of atomic force microscopy and sub-micrometer focused X-ray techniques

2014 ◽  
Vol 1712 ◽  
Author(s):  
Thomas W. Cornelius ◽  
Zhe Ren ◽  
Francesca Mastropietro ◽  
Simon Langlais ◽  
Anton Davydok ◽  
...  
Keyword(s):  
Mechanical Response ◽  
Elemental Distribution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cu Nanowires ◽  
Force Microscopy ◽  
Indentation Tests ◽  
Scanning Force ◽  
Diffraction Patterns

ABSTRACTA scanning force microscope for in situ nanofocused X-ray studies (SFINX) has been developed which can be installed on diffractometers at synchrotron beamlines allowing for the combination with various techniques such as coherent X-ray diffraction and fluorescence. The capabilities of this device are demonstrated on Cu nanowires and on Au islands grown on sapphire (0001). The sample topography, crystallinity, and elemental distribution of the same area are investigated by recording simultaneously an AFM image, a scanning X-ray diffraction map, and a fluorescence map. Additionally, the mechanical response of Au islands is studied by in situ indentation tests employing the AFM-tip and recording 2D X-ray diffraction patterns during mechanical loading.

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