A Comparison of Commercially Available Screen-Printed Electrodes for Electrogenerated Chemiluminescence Applications

We examined a series of commercially available screen-printed electrodes (SPEs) for their suitability for electrochemical and electrogenerated chemiluminescence (ECL) detection systems. Using cyclic voltammetry with both a homogeneous solution-based and a heterogeneous bead-based ECL assay format, the most intense ECL signals were observed from unmodified carbon-based SPEs. Three commercially available varieties were tested, with Zensor outperforming DropSens and Kanichi in terms of sensitivity. The incorporation of nanomaterials in the electrode did not significantly enhance the ECL intensity under the conditions used in this evaluation (such as gold nanoparticles 19%, carbon nanotubes 45%, carbon nanofibers 21%, graphene 48%, and ordered mesoporous carbon 21% compared to the ECL intensity of unmodified Zensor carbon electrode). Platinum and gold SPEs exhibited poor relative ECL intensities (16% and 10%) when compared to carbonaceous materials, due to their high rates of surface oxide formation and inefficient oxidation of tri-n-propylamine (TPrA). However, the ECL signal at platinum electrodes can be increased ∼3-fold with the addition of a surfactant, which enhanced TPrA oxidation due to increasing the hydrophobicity of the electrode surface. Our results also demonstrate that each SPE should only be used once, as we observed a significant change in ECL intensity over repeated CV scans and SPEs cannot be mechanically polished to refresh the electrode surface.

How the anisotropy of surface oxide formation influences the transient activity of a surface reaction

Scanning photoelectron microscopy (SPEM) and photoemission electron microscopy (PEEM) allow local surface analysis and visualising ongoing reactions on a µm-scale. These two spatio-temporal imaging methods are applied to polycrystalline Rh, representing a library of well-defined high-Miller-index surface structures. The combination of these techniques enables revealing the anisotropy of surface oxidation, as well as its effect on catalytic hydrogen oxidation. In the present work we observe, using locally-resolved SPEM, structure-sensitive surface oxide formation, which is summarised in an oxidation map and quantitatively explained by the novel step density (SDP) and step edge (SEP) parameters. In situ PEEM imaging of ongoing H2 oxidation allows a direct comparison of the local reactivity of metallic and oxidised Rh surfaces for the very same different stepped surface structures, demonstrating the effect of Rh surface oxides. Employing the velocity of propagating reaction fronts as indicator of surface reactivity, we observe a high transient activity of Rh surface oxide in H2 oxidation. The corresponding velocity map reveals the structure-dependence of such activity, representing a direct imaging of a structure-activity relation for plenty of well-defined surface structures within one sample.

Investigation of Oxidation Behavior of 304L and 310S Steels with Potential Application in Supercritical Water-cooled Nuclear Reactors

Selecting proper candidate materials is one key issue for the development of the supercritical water-cooled nuclear reactor (SCWR). Designing or choosing the most fitting materials means better sustainability, economics and safety. As the supercritical water is a very aggressive corrosive media, corrosion becomes one challenging problem for the materials used in the SCWR. This paper involves the corrosion testing of two stainless steels (304L and 310S) and microstructure evaluation of samples after being exposed to supercritical water. The test parameters were set at the temperature of 550oC and the pressure of 25 MPa for up to 63 days. The samples were investigated using gravimetric corrosion test, optical microscopy, scanning electron microscopy coupled with energy dispersive X-ray spectroscopy. Results showed a lower corrosion performance, in terms of weight change and surface oxide formation, for 304L due to its low chromium content. 310S has excellent corrosion resistance because the chromium content is higher. The results obtained will be useful in future research of test protocol and development of alloys that could be used as reactor fuel cladding and other components in the SCWR.

Oxygen Evolution Reaction at IrO2/Ir(Ni) Film Electrodes Prepared by Galvanic Replacement and Anodization: Effect of Precursor Ni Film Thickness

IrO2/Ir(Ni) film electrodes of variable Ni content have been prepared via a galvanic replacement method, whereby surface layers of pre-deposited Ni are replaced by Ir, followed by electrochemical anodization. Electrodeposition of Ni on a glassy carbon electrode support has been carried out at constant potential and the charge of electrodeposited Ni controlled so as to investigate the effect of precursor Ni layer thickness on the electrocatalytic activity of the corresponding IrO2/Ir(Ni)/GC electrodes for the oxygen evolution reaction (OER). After their preparation, these electrodes were characterized by microscopic (SEM) and spectroscopic (EDS, XPS) techniques, revealing the formation of Ir deposits on the Ni support and a thin IrO2 layer on their surfaces. To determine the electroactive surface area of the IrO2 coatings, cyclic voltammograms were recorded in the potential range between hydrogen and oxygen evolution and the charge under the anodic part of the curves, corresponding to Ir surface oxide formation, served as an indicator of the quantity of active IrO2 in the film. The electrocatalytic activity of the coatings for OER was investigated by current–potential curves under steady state conditions, revealing that the catalysts prepared from thinner Ni films exhibited enhanced electrocatalytic performance.

Evidence of the O–Pd–O and Pd–O4 structure units as oxide seeds and their origin on Pd(211): revealing the mechanism of surface oxide formation

The formation of surface oxides on metal surfaces is not only important in materials science, but also of significance in heterogeneous catalysis due to the fact that during most oxidation reactions the metal catalysts are inevitably oxidized, which may cause dramatic consequences in the reactions.

Imaging the confined surface oxidation of Ni3Al(111) by in situ high temperature scanning tunneling microscopy

Surface oxide growth ontop of Ni3Al(111) upon O2 exposure at 735 K leads to both, overgrowth of steps and terrace retraction (blue lines indicate the initial step edge positions). The material transport during surface oxide formation appears when subtracting high temperature scanning tunneling microscopy images one from another.