scholarly journals Electrochemical flow cell enabling operando probing of electrocatalyst surfaces by X-ray spectroscopy and diffraction

2019 ◽  
Vol 21 (10) ◽  
pp. 5402-5408 ◽  
Author(s):  
Maryam Farmand ◽  
Alan T. Landers ◽  
John C. Lin ◽  
Jeremy T. Feaster ◽  
Jeffrey W. Beeman ◽  
...  
Keyword(s):  
Mass Transport ◽  
Catalyst Surface ◽  
Grazing Incidence ◽  
Flow Cell ◽  
High Current ◽  
X Ray ◽  
Current Operation ◽  
Electrochemical Flow Cell

Grazing incidence cell probes catalyst surface during high current operation with improved mass transport.

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 ◽  
...  
Keyword(s):  
Flow Cell ◽  
X Ray ◽  
Electrochemical Flow Cell

A flow cell for transient voltammetry and in situ grazing incidence X-ray diffraction characterization of electrocrystallized cadmium(II) tetracyanoquinodimethane

2011 ◽  
Vol 56 (3) ◽  
pp. 1546-1553 ◽  
Author(s):  
Jean-Pierre Veder ◽  
Ayman Nafady ◽  
Graeme Clarke ◽  
Ross P. Williams ◽  
Roland De Marco ◽  
...  
Keyword(s):  
Grazing Incidence ◽  
Flow Cell ◽  
X Ray Diffraction ◽  
X Ray

In situsynchrotron X-ray diffraction investigation of the evolution of a PbO2/PbSO4surface layer on a copper electrowinning Pb anode in a novel electrochemical flow cell

2015 ◽  
Vol 22 (2) ◽  
pp. 366-375 ◽  
Author(s):  
Marie Clancy ◽  
Mark J. Styles ◽  
Colleen J. Bettles ◽  
Nick Birbilis ◽  
Miao Chen ◽  
...  
Keyword(s):  
Flow Cell ◽  
Quantitative Phase Analysis ◽  
X Ray Diffraction ◽  
Pure Lead ◽  
X Ray ◽  
Copper Electrowinning ◽  
Number Of Cycles ◽  
Kinetics Of ◽  
Electrochemical Flow Cell

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.

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

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

An ultra-high vacuum electrochemical flow cell for in situ/operando soft X-ray spectroscopy study

2014 ◽  
Vol 85 (4) ◽  
pp. 043106 ◽  
Author(s):  
Debajeet K. Bora ◽  
Per-Anders Glans ◽  
John Pepper ◽  
Yi-Sheng Liu ◽  
Chun Du ◽  
...  
Keyword(s):  
High Vacuum ◽  
Flow Cell ◽  
Ultra High Vacuum ◽  
Spectroscopy Study ◽  
X Ray ◽  
Electrochemical Flow Cell

scholarly journals Novel micro-reactor flow cell for investigation of model catalysts usingin situgrazing-incidence X-ray scattering

2016 ◽  
Vol 23 (2) ◽  
pp. 455-463 ◽  
Author(s):  
Jan Kehres ◽  
Thomas Pedersen ◽  
Federico Masini ◽  
Jens Wenzel Andreasen ◽  
Martin Meedom Nielsen ◽  
...  
Keyword(s):  
Grazing Incidence ◽  
Flow Cell ◽  
Reaction Chamber ◽  
Silicon On Insulator ◽  
X Ray ◽  
Ru Nanoparticles ◽  
X Ray Scattering ◽  
Micro Reactor ◽  
Ray Scattering

The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performingin situgrazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS).In situexperiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneousin situGISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles.

scholarly journals In situsynchrotron X-ray diffraction investigation of the evolution of a PbO2/PbSO4surface layer on a copper electrowinning Pb anode in a novel electrochemical flow cell. Corrigendum

2015 ◽  
Vol 22 (3) ◽  
pp. 863-864
Author(s):  
Marie Clancy ◽  
Mark J. Styles ◽  
Colleen J. Bettles ◽  
Nick Birbilis ◽  
Miao Chen ◽  
...  
Keyword(s):  
Flow Cell ◽  
X Ray Diffraction ◽  
X Ray ◽  
Copper Electrowinning ◽  
Electrochemical Flow Cell

Figures 7 and 8 of the article by Clancyet al.[(2015),J. Synchrotron Rad.22, 366–375] are corrected.

Spatial resolution of X-ray microanalysis in thin foils

1978 ◽  
Vol 36 (1) ◽  
pp. 544-545
Author(s):  
R. Hutchings ◽  
I.P. Jones ◽  
M.H. Loretto ◽  
R.E. Smallman
Keyword(s):  
Spatial Resolution ◽  
Electron Probe ◽  
Beam Divergence ◽  
Inelastic Interaction ◽  
Specimen Thickness ◽  
High Current ◽  
Beam Spreading ◽  
X Ray ◽  
Thin Foils ◽  
Complex Calculation

There is increasing interest in X-ray microanalysis of thin specimens and the present paper attempts to define some of the factors which govern the spatial resolution of this type of microanalysis. One of these factors is the spreading of the electron probe as it is transmitted through the specimen. There will always be some beam-spreading with small electron probes, because of the inevitable beam divergence associated with small, high current probes; a lower limit to the spatial resolution is thus 2αst where 2αs is the beam divergence and t the specimen thickness.In addition there will of course be beam spreading caused by elastic and inelastic interaction between the electron beam and the specimen. The angle through which electrons are scattered by the various scattering processes can vary from zero to 180° and it is clearly a very complex calculation to determine the effective size of the beam as it propagates through the specimen.

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