scholarly journals Electrochemical Flow-Cell Setup for In Situ X-ray Investigations

2016 ◽  
Vol 163 (10) ◽  
pp. H906-H912 ◽  
Author(s):  
Tobias Binninger ◽  
Emiliana Fabbri ◽  
Alexandra Patru ◽  
Marios Garganourakis ◽  
Jun Han ◽  
...  
2015 ◽  
Vol 22 (2) ◽  
pp. 366-375 ◽  
Author(s):  
Marie Clancy ◽  
Mark J. Styles ◽  
Colleen J. Bettles ◽  
Nick Birbilis ◽  
Miao Chen ◽  
...  

This paper describes the quantitative measurement, byin situsynchrotron X-ray diffraction (S-XRD) and subsequent Rietveld-based quantitative phase analysis and thickness calculations, of the evolution of the PbO2and PbSO4surface layers formed on a pure lead anode under simulated copper electrowinning conditions in a 1.6 MH2SO4electrolyte at 318 K. This is the first report of a trulyin situS-XRD study of the surface layer evolution on a Pb substrate under cycles of galvanostatic and power interruption conditions, of key interest to the mining, solvent extraction and lead acid battery communities. The design of a novel reflection geometry electrochemical flow cell is also described. Thein situS-XRD results show that β-PbO2forms immediately on the anode under galvanostatic conditions, and undergoes continued growth until power interruption where it transforms to PbSO4. The kinetics of the β-PbO2to PbSO4conversion decrease as the number of cycles increases, whilst the amount of residual PbO2increases with the number of cycles due to incomplete conversion to PbSO4. Conversely, complete transformation of PbSO4to β-PbO2was observed in each cycle. The results of layer thickness calculations demonstrate a significant volume change upon PbSO4to β-PbO2transformation.


2016 ◽  
Vol 163 (10) ◽  
pp. H913-H920 ◽  
Author(s):  
Jérémy Tillier ◽  
Tobias Binninger ◽  
Marios Garganourakis ◽  
Alexandra Patru ◽  
Emiliana Fabbri ◽  
...  

2014 ◽  
Vol 85 (4) ◽  
pp. 043106 ◽  
Author(s):  
Debajeet K. Bora ◽  
Per-Anders Glans ◽  
John Pepper ◽  
Yi-Sheng Liu ◽  
Chun Du ◽  
...  

2011 ◽  
Vol 56 (3) ◽  
pp. 1546-1553 ◽  
Author(s):  
Jean-Pierre Veder ◽  
Ayman Nafady ◽  
Graeme Clarke ◽  
Ross P. Williams ◽  
Roland De Marco ◽  
...  

2008 ◽  
Vol 41 (5) ◽  
pp. 918-929 ◽  
Author(s):  
Andrew J. Allen ◽  
Vincent A. Hackley ◽  
Pete R. Jemian ◽  
Jan Ilavsky ◽  
Joan M. Raitano ◽  
...  

Results are presented for anin situsynchrotron-based ultra-small-angle X-ray scattering (USAXS) study of the solution-mediated formation and growth of nanocrystalline ceria (n-CeO2) using a new remote-controlled, isothermal, circulating fluid flow cell. The fluid flow mitigates or reduces X-ray beam-induced damage, air bubbles or particulate flocculation within the bulk solution, but prevents any coarse particulates that do form from settling out from suspension. Combined with the large-scale range accessible in USAXS studies, the flow cell has enabled measurement,in situand in real time, of structural characteristics from 10 Å to a few micrometres in size as a function of the changing physical and chemical conditions. By applying a multi-component model, the nanoparticle formation and growth component has been identified. Control and online monitoring of flow rate, temperature and pH suspension conditions have permitted real-time studies of the formation and growth of the individual n-CeO2particles from homogeneous dilute solution over several hours. Aspects of the nanoparticle nucleation and growth are revealed that have not been observed directly in measurements on this system.


2020 ◽  
Author(s):  
Jeroen F. Van Stappen ◽  
Maartje E. Houben ◽  
Timotheus K.T. Wolterbeek ◽  
Alessandro Tengattini ◽  
Takahiro Shinohara ◽  
...  

<p>Subsurface activities, such as energy production or geo-storage, affect the natural equilibrium of the reservoir and surrounding geological system. Fluid production from porous sandstones, for example, is often associated with reservoir compaction and induced seismicity, such as seen in the Groningen Gas Field. Production-induced stress changes lead to compaction by elastic and inelastic mechanisms. Partitioning between elastic and inelastic processes control the energy budget available for driving seismogenic events. To predict the amount of inelastic strain, it is key to identify the microscopic mechanisms controlling it. One of the current hypotheses is that micro-strains are accommodated by localized compaction of inter-granular clay films. In contrast to sandstones, claystones offer potential both as source rocks for shale gas and containment for the storage of radioactive waste and CO<sub>2</sub>. It is known that fluid flow in intact and fractured claystones is slow due to pore throats below 10 nm. However, it is unclear whether fractured shales contain a hierarchy of multi-scale highways and byways for fluid transport that is either poorly connected or more easily cross-linked and stable under in-situ conditions. Depending on how fractures change due to in-situ conditions, the shales may have a high potential as barriers in geo-storage systems, or they are of interest in relation to energy production.</p><p>This leads to two widely different research questions:</p><ul><li>How do sandstones compact due to changing stress conditions?</li> <li>How do fractures influence fluid flow in shales under in-situ stress conditions?</li> </ul><p>Despite the distance between these research questions, both can be addressed using in-situ imaging. We have developed a compaction cell and a fluid flow cell to perform experiments at the D50/NeXT beamline of the Institut Laue-Langevin in Grenoble, France. Here, combined X-ray and neutron imaging is possible.</p><p>With the compaction cell, sandstone samples from the Groningen gas field were uniaxially compacted to axial stresses of 45 MPa. At different intervals, 3D neutron and X-ray computed tomography scans were taken. As such, 4D representations (3D volumetric + time) of the in-situ changes were obtained using both neutron and X-ray tomography. The X-ray imaging allows a thorough inspection of the grain-scale deformation of the sample, while the neutron imaging highlights the changes in porosity and gives an indication of the role of clay films.</p><p>With the fluid flow cell, fractured samples of the Whitby mudstone were subjected to fluid flow under different hydrostatic pressures. The flow path evolution within the sample was visualized using neutron radiography, giving an indication of the differences between fracture and matrix permeability.</p><p>In this contribution, we will show preliminary results of four experiments performed at the D50/NeXT beamline in October 2019. We will discuss the applicability of using neutron imaging to study grain-scale processes occurring in compacting sandstone, as well as for understanding the fluid pathways in clay-rich shales, with direct implications for energy production and geo-storage.</p>


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