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 ◽  
...  

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.

2018 ◽  
Vol 51 (3) ◽  
pp. 796-801 ◽  
Author(s):  
Kouji Sakaki ◽  
Hyunjeong Kim ◽  
Akihiko Machida ◽  
Tetsu Watanuki ◽  
Yoshinori Katayama ◽  
...  

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.


2006 ◽  
Vol 971 ◽  
Author(s):  
Koya Okudera ◽  
Koichi Hamada ◽  
Takanori Suda ◽  
Naoyuki Hashimoto ◽  
Somei Ohnuki ◽  
...  

ABSTRACTHigh-resolution and “environmental cell” microscopy were applied for surveying the reaction of hydrides in Vanadium and Magnesium based alloys, which are candidate for hydrogen storage materials of advanced hydrogen energy systems. For clarify the hydrogenation process, in-situ experiment was carried out by using 200 kV TEM equipped with a newly developed environmental cell, which is enable to observe transmitted image and electron-diffraction under gas reaction under hydrogen environment of 0.1 MPa at room temperature. In case of Vanadium, bending fringe was created under hydrogen-gas of 0.1 MPa, which means that hydrogen reaction is not so quick in this case, and the local stress due to the hydrogen solution caused the fringes. In case of Magnesium, the gas reacted with the powders and showed the swelling, where the surface steps with several ten nm become to more straight, and also SADP showed the formation of MgH2. In-situ experiment for hydrogenation reaction by using the environmental cell has started recently, therefore the precise studies will be continued, as well as its improvement, especially in the transparence films.


2019 ◽  
Vol 3 (4) ◽  
pp. 956-964 ◽  
Author(s):  
Jun Sugiyama ◽  
Izumi Umegaki ◽  
Mitsuru Matsumoto ◽  
Kazutoshi Miwa ◽  
Hiroshi Nozaki ◽  
...  

To study the mechanism determining the desorption temperature of hydrogen storage materials, we have measured muon spin rotation and relaxation (μ+SR) in MgH2 together with the pressure in the sample space.


2012 ◽  
Vol 45 (5) ◽  
pp. 902-905 ◽  
Author(s):  
Roxana Flacau ◽  
Jim Bolduc ◽  
Thomas Bibienne ◽  
Jacques Huot ◽  
Helmut Fritzsche

In situneutron powder diffraction (NPD) measurements of hydrogenation processes taking place at high temperatures pose difficulties related to the choice of sample can material. This article describes a simple design for a copper-coated vanadium can and its connection to the gas-handling system, tested up to 523 K. High-quality NPD patterns of TiV1.2Mn0.8body-centred cubic alloy, as-cast and partially hydrogenated, were collected at 373 K and deuterium pressures up to 2 bar (200 kPa).


2015 ◽  
Vol 3 (16) ◽  
pp. 8294-8299 ◽  
Author(s):  
Yi Jia ◽  
Chenghua Sun ◽  
Ye Peng ◽  
Wenqi Fang ◽  
Xuecheng Yan ◽  
...  

The facile and scalable fabrication of ultrafine (<5 nm) nanoparticles (NPs) as effective catalysts is the key for enhancing the kinetics of most hydrogen storage materials (HSMs).


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