scholarly journals Detection and quantification of defect evolution at buried metal-oxide-polymer interface on rough substrate by local electrochemical impedance mapping

2021 ◽  
pp. 138467
Author(s):  
Thomas Sanchez ◽  
Ekaterina Kurchavova ◽  
Viacheslav Shkirskiy ◽  
Jolanta Swiatowska ◽  
Vincent Vivier ◽  
...  
Catalysts ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 968 ◽  
Author(s):  
Lutho Klaas ◽  
Mmalewane Modibedi ◽  
Mkhulu Mathe ◽  
Huaneng Su ◽  
Lindiwe Khotseng

This study investigates the most effective electrocatalyst for glycerol oxidation reaction (GOR) in alkaline medium for five synthesized electrocatalysts, Pd, PdNi, PdNiO, PdMn3O4 and PdMn3O4NiO, supported on multi-walled carbon nanotubes (MWCNTs) prepared using the polyol method. The particle size and crystalline size of the electrocatalysts were determined using HR-TEM and XRD techniques, respectively, while EDS was used to determine the elemental composition. XRD showed crystalline sizes ranging from 3.4 to 10.1 nm, while HR-TEM revealed particle sizes within the range of 3.4 and 7.2 nm. The electroactivity, electron kinetics and stability of the electrocatalysts towards glycerol in alkaline medium was evaluated using linear sweep voltammetry (LSV), electrochemical impedance spectroscopy (EIS) and chronoamperometry (CA), respectively, while the electroactive surface area (ECSA) of the electrocatalysts was determined using cyclic voltammetry (CV). The metal oxide-based Pd electrocatalysts PdNiO and PdMn3O4 were the most electrochemically active, while the addition of the second metal oxide to the Pd electrocatalyst PdMn3O4NiO did not show any improvement. This was associated with this electrocatalyst having the highest particle and crystalline sizes.


2012 ◽  
Vol 1383 ◽  
Author(s):  
Chris R. M. Grovenor ◽  
Na Ni ◽  
Daniel Hudson ◽  
Sean S. Yardley ◽  
Katie L. Moore ◽  
...  

ABSTRACTAqueous corrosion of zirconium alloys has become the major factor limiting prolonged fuel campaigns in nuclear plant. Studies using SEM, TEM and electrochemical impedance measurements have been interpreted as showing a dense inner-most oxide layer, and an increased thickness of the layer has been correlated to a better corrosion resistance. Many authors have reported that an ‘intermediate layer’ at the metal oxide interface has a complex structure or/and stochiometry different to that of both the bulk oxide and bulk metal, sometimes claimed to be a suboxide phase. Diffraction evidence has suggested the presence of both cubic ZrO and rhombohedral Zr3O phases, and compositional analysis has revealed similar variations in local oxygen stoichiometry.We have carried out a systematic investigation of the structure and chemistry of the metal/oxide interface in samples of commercial ZIRLO corroded for times up to 180 days. We have developed new experimental techniques for the study of these interfaces both by Electron Energy Loss Spectroscopy (EELS) analysis in the Transmission Electron Microscope (TEM) and by Atom Probe Tomography (APT), and exactly the same samples have been investigated by both techniques. Our results show the development of a clearly defined suboxide layer of stoichiometry close to ZrO, and the subsequent disappearance of this layer at the first of the characteristic ‘breakaway’ transitions in the oxidation kinetics. We can correlate this behaviour with changes in the structure of the oxide layer, and particularly the development of interconnected porosity that links the corroding interface with the aqueous environment. Using high resolution SIMS analysis of isotopically spiked samples we demonstrate the penetration of the oxidising species through these porous outer oxide layers.


2016 ◽  
Vol 3 (7) ◽  
pp. 1500616 ◽  
Author(s):  
Yunus Sevinchan ◽  
Paul E. Hopkinson ◽  
Artem A. Bakulin ◽  
Julia Herz ◽  
Marcus Motzkus ◽  
...  

2016 ◽  
Vol 3 (7) ◽  
Author(s):  
Yunus Sevinchan ◽  
Paul E. Hopkinson ◽  
Artem A. Bakulin ◽  
Julia Herz ◽  
Marcus Motzkus ◽  
...  

Author(s):  
David A. Brewster ◽  
Melissa D. Koch ◽  
Kathryn E Knowles

This paper describes analysis of dropcast nanocrystalline and electrochemically deposited films of NiO and α-Fe2O3 as model metal oxide semiconductors immersed in redox-inactive organic electrolyte solutions using electrochemical impedance spectroscopy...


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