Development of an electrochemical procedure for monitoring hydrogen sorption/desorption in steel

Hydrogen embrittlement leads to mechanical degradation of metals. Hence, hydrogen sorption/desorption properties of metals need to be characterized. An electrochemical procedure based on cyclic voltammetry (CV) and potentiostatic polarization is elaborated on plain-carbon steel. The procedure consists of first two consecutive CV cycles (pretreatment and reference CV), followed by cathodic H-charging, and subsequent CV scans to study and quantify the H-sorption/desorption. Best practice in this procedure is to perform all steps consecutively without interruption or sample manipulations between steps to avoid spontaneous H-loss. The H-related interaction with the steel is clearly identified in the CV and can be differentiated from the electrolyte contribution coming from thiourea. The study confirms the role of thiourea as H-recombination poison in alkaline solution, and also demonstrates that it contributes to the CV response. Additionally, various charging times are investigated to study the time to H-saturation, and also the scan rate during the CV procedure is varied to study time-related phenomena. Dedicated discharging experiments were included in the study to complement the CV data, giving additional insights in the H-steel interaction. Moreover, hydrogen related findings are successfully verified by using a complimentary method, i.e. hot extraction. The better understanding of the peaks in the CV and the continuous procedure result in a reliable methodology to characterize the H-sorption/desorption in steel

Patterning of graphene on silicon-on-insulator waveguides through laser ablation and plasma etching

We present the use of femtosecond laser ablation for the removal of monolayer graphene from silicon-on-insulator (SOI) waveguides, and the use of oxygen plasma etching through a metal mask to peel off graphene from the grating couplers attached to the waveguides. Through Raman spectroscopy and atomic force microscopy, we show that the removal of graphene is successful with minimal damage to the underlying SOI waveguides. Finally, we employ both removal techniques to measure the contribution of graphene to the loss of grating-coupled graphene-covered SOI waveguides using the cut-back method. This loss contribution is measured to be 0.132 dB/μm

Doped ordered mesoporous carbons as novel, selective electrocatalysts for the reduction of nitrobenzene to aniline

Ordered mesoporous carbons (OMCs) doped with nitrogen, phosphorus or boron were synthesised through a two-step nanocasting method and studied as electrocatalysts for the reduction of nitrobenzene to aniline in a half-cell setup. The nature of the dopant played a crucial role in the electrocatalytic performance of the doped OMCs, which was monitored by LSV with a rotating disk electrode setup. The incorporation of boron generated the electrocatalysts with the highest kinetic current density, whereas the incorporation of phosphorus led to the lowest overpotential. Doping with nitrogen led to intermediate behaviour in terms of onset potential and kinetic current density, but provided the highest selectivity towards aniline, thus resulting in the most promising electrocatalyst developed in this study. Density functional theory calculations allowed explaining the observed difference in the onset potentials between the various doped OMCs, and indicated that both graphiticN and pyrdinic N can generate active sites in the N-doped electrocatalyst. A chronoamperometric experiment over N-doped OMC performed at -0.75 V vs. Fc/Fc(+) in an acidic environment, resulted in a conversion of 61% with an overall selectivity of 87% to aniline. These are the highest activity and selectivity ever reported for an electrocatalyst for the reduction of nitrobenzene to aniline, making N-doped OMC a promising candidate for the electrochemical cogeneration of this industrially relevant product and electricity in a fuel cell setup

Effect of hydrogen peroxide on bovine serum albumin adsorption on Ti6Al4V alloy: A scanning Kelvin probe force microscopy study

Abstract Protein adsorption on the surface of implant materials greatly affects the performance of the implants, such as their stability as well as the release of metal ions from and the adhesion of cells to their surface. In addition, the production of extracellular H2O2 from the activation of inflammatory cells could interfere with protein–metal interactions and/or modify the conformation of adsorbed proteins. In this study, we utilised scanning Kelvin probe force microscopy (SKPFM) to visualise the impact of H2O2 on bovine serum albumin (BSA) adsorption on the positively polarised Ti6Al4V alloy in a phosphate-buffered saline (PBS) solution. We show that the negatively charged BSA adsorbs onto the surface of polished and anodically polarised Ti6Al4V in a dense layer with a continuous network-like morphology or cluster shape and reduces the variation in the total surface potential compared to that of blank Ti6Al4V. However, addition of H2O2 to the PBS solution interferes with the formation of the dense protein network, and only a thin and discontinuous protein layer adsorbs onto the surface of the Ti6Al4V alloy, lowering the total surface potential difference. The information presented in this work provides new insights into the adsorption distribution of proteins on metallic substrates in biomaterials field

Corrosion protection of Cu by atomic layer deposition

Atomic layer deposition (ALD) is a vapor phase technique that is able to deposit uniform, conformal thin films with an excellent thickness control at the atomic scale. 18 nm thick Al2O3 and TiO2 coatings were deposited conformaly and pinhole-free onto micrometer-sized Cu powder, using trimethylaluminum and tetrakis(dimethylamido)titanium(IV), respectively, as a precursor and de-ionized water as a reactant. The capability of the ALD coating to protect the Cu powder against corrosion was investigated. Therefore, the stability of the coatings was studied in solutions with different pH in the range of 0-14, and in situ raman spectroscopy was used to detect the emergence of corrosion products of Cu as an indication that the protective coating starts to fail. Both ALD coatings provide good protection at standard pH values in the range of 5-7. In general, the TiO2 coating shows a better barrier protection against corrosion than the Al2O3 coating. However, for the most extreme pH conditions, pH 0 and pH 14, the TiO2 coating starts also to degrade. Published by the AVS

Morphology and Microstructure Evolution of Gold Nanostructures in the Limited Volume Porous Matrices

The modern development of nanotechnology requires the discovery of simple approaches that ensure the controlled formation of functional nanostructures with a predetermined morphology. One of the simplest approaches is the self-assembly of nanostructures. The widespread implementation of self-assembly is limited by the complexity of controlled processes in a large volume where, due to the temperature, ion concentration, and other thermodynamics factors, local changes in diffusion-limited processes may occur, leading to unexpected nanostructure growth. The easiest ways to control the diffusion-limited processes are spatial limitation and localized growth of nanostructures in a porous matrix. In this paper, we propose to apply the method of controlled self-assembly of gold nanostructures in a limited pore volume of a silicon oxide matrix with submicron pore sizes. A detailed study of achieved gold nanostructures' morphology, microstructure, and surface composition at different formation stages is carried out to understand the peculiarities of realized nanostructures. Based on the obtained results, a mechanism for the growth of gold nanostructures in a limited volume, which can be used for the controlled formation of nanostructures with a predetermined geometry and composition, has been proposed. The results observed in the present study can be useful for the design of plasmonic-active surfaces for surface-enhanced Raman spectroscopy-based detection of ultra-low concentration of different chemical or biological analytes, where the size of the localized gold nanostructures is comparable with the spot area of the focused laser beam

Screening and classification of ordinary chondrites by Raman spectroscopy

Classification of ordinary chondrite meteorites generally implies (1) determining the chemical group by the composition in endmembers of olivine and pyroxene, and (2) identifying the petrologic group by microstructural features. The composition of olivine and pyroxene is commonly obtained by microprobe analyses or oil immersion of mineral separates. We propose Raman spectroscopy as an alternative technique to determine the endmember content of olivine and pyroxene in ordinary chondrites, by using the link between the wavelength shift of selected characteristic peaks in the spectra of olivine and pyroxene and the Mg/Fe ratio in these phases. The existing correlation curve has been recalculated from the Raman spectrum of reference minerals of known composition and further refined for the range of chondritic compositions. Although the technique is not as accurate as the microprobe for determining the composition of olivine and pyroxene, for most of the samples the chemical group can be easily determined by Raman spectroscopy. Blind tests with ordinary chondrites of different provenance, weathering, and shock stages have confirmed the potential of the method. Therefore, we suggest that a preliminary screening and the classification of most of the equilibrated ordinary chondrites can be carried out using an optical microscope equipped with a Raman spectrometer.SCOPUS: ar.jFLWINinfo:eu-repo/semantics/publishe

In Search of Neoproterozoic Fungi Microfossils

info:eu-repo/semantics/nonPublishe