Search Results (6)

X-ray photoelectron spectroscopy (XPS) technology is extensively applied in the field of catalysts, offering deep insights into their electronic structures and chemical composition. The development of advanced techniques based on XPS instrumentation allows for a deeper and more holistic exploration of the characteristics of catalytic materials. This mini-review introduces and summarizes the primary applications of XPS-based analysis methods, including ion scattering spectroscopy (ISS) for analyzing single atomic layers, angle-resolved XPS, high energy X-ray sources and argon ion sputtering, each providing different depths of information about a sample. It also summarizes the use of inert atmosphere transfer devices and high-temperature reactors for quasi in situ monitoring as well as the integration of in situ techniques, including light irradiation XPS, to study catalysts’ behavior under realistic conditions. Full article

The state of Sonora, Mexico, stands as one of the leading producers of pecan nuts in the country, which are commercialized without shells, leaving behind this unused residue. Additionally, this region has abundant solar resources, as shown by its high levels of direct normal irradiance (DNI). This study contributes to research efforts aimed at achieving a synergy between concentrated solar energy technology and biomass pyrolysis processes, with the idea of using the advantages of organic waste to reduce greenhouse gas emissions and avoiding the combustion of conventional pyrolysis through the concentration of solar thermal energy. The objective of this study is to pioneer a new experimental analysis methodology in research on solar pyrolysis reactors. The two main features of this new methodology are, firstly, the comparison of temperature profiles during the heating of inert and reactive materials and, secondly, the analysis of heating rates. This facilitated a better interpretation of the observed phenomenon. The methodology encompasses two different thermal experiments: (A) the pyrolysis of pecan shells and (B) the heating–cooling process of the biochar produced in experiment (A). Additionally, an experiment involving the heating of volcanic stone is presented, which reveals the temperature profiles of an inert material and serves as a comparative reference with experiment (B). In this experimental study, 50 g of pecan shells were subjected to pyrolysis within a cylindrical stainless-steel reactor with a volume of 156 cm³, heated by concentrated radiation from a solar simulator. Three different heat fluxes were applied (234, 482, and 725 W), resulting in maximum reaction temperatures of 382, 498, and 674 °C, respectively. Pyrolysis gas analyses (H₂, CO, CO₂, and CH₄) and characterization of the obtained biochar were conducted. The analysis of heating rates, both for biochar heating and biomass pyrolysis, facilitated the identification, differentiation, and interpretation of processes such as moisture evaporation, tar production endpoint, cellulosic material pyrolysis, and lignin degradation. This analysis proved to be a valuable tool as it revealed heating and cooling patterns that were not previously identified. The potential implications of this tool would be associated with improvements in the design and operation protocols of solar reactors. Full article

The quasi-steady flow assumption (QSFA) is commonly used in the field of biomechanics of phonation. It approximates time-varying glottal flow with steady flow solutions based on frozen glottal shapes, ignoring unsteady flow behaviors and vocal fold motion. This study examined the limitations of QSFA in human phonation using numerical methods by considering factors of phonation frequency, air inertance in the vocal tract, and irregular glottal shapes. Two sets of irregular glottal shapes were examined through dynamic, pseudo-static, and quasi-steady simulations. The differences between dynamic and quasi-steady/pseudo-static simulations were measured for glottal flow rate, glottal wall pressure, and sound spectrum to evaluate the validity of QSFA. The results show that errors in glottal flow rate and wall pressure predicted by QSFA were small at 100 Hz but significant at 500 Hz due to growing flow unsteadiness. Air inertia in the vocal tract worsened predictions when interacting with unsteady glottal flow. Flow unsteadiness also influenced the harmonic energy ratio, which is perceptually important. The effects of glottal shape and glottal wall motion on the validity of QSFA were found to be insignificant. Full article

The electrochemical behavior of dysprosium ions, as well as dysprosium and nickel ion co-reduction, on inert tungsten electrodes and active nickel electrodes were studied in the eutectic KCl-NaCl-CsCl melt at a temperature of 823 K using the methods of cyclic and square-wave voltammetry and open circuit chronopotentiometry. The process of Dy³⁺ ions electroreduction was found to be reversible and to proceed within a single three-electron stage up to the polarization rate of 0.1 V/s. The increase in the polarization rate indicates a slower rate of the charge transfer, which causes the quasi-reversible character of the charge transfer. It is shown that when the KCl-NaCl-CsCl eutectic melt contains both nickel and dysprosium ions, the voltammetry curves at 823 K have a wave of nickel ion reduction at the potentials of −(0.22–0.28) V and a dysprosium ion reduction at the potentials of −(2.175–2.250) V relative to a chlorine-silver reference electrode. Apart from these waves, the voltammograms have two reduction waves at the potentials of −(1.9–1.95) V and −(2.05–2.1) V. These waves are associated with the reduction of dysprosium ions and their depolarization on metallic nickel, which was preliminary deposited on the tungsten electrode, as well as the formation of the intermetallic phases of dysprosium and nickel of various Dy_xNi_y compositions. The (E-t) dependencies of the open circuit chronopotentiometry elucidate plateaus of the potential delay, which correspond to the dissolution of separate dysprosium and nickel intermetallic phases. Based on the results of the voltammetry changes and the chronopotentiometry of the open circuit, a series of electrochemical syntheses were performed in the potentiostatic regime at the potentials of −(1.7–2.1) V. The intermetallic phases of DyNi₅, DyNi₃ and DyNi₂ were obtained at a definite ratio of the dysprosium and nickel chloride concentrations in the KCl-NaCl-CsCl eutectic melt and at a temperature of 823 K. The synthesized intermetallic samples were characterized by X-ray diffraction and scanning electron microscopy. Full article

Synthesis atmosphere (i.e., air and nitrogen) effects on the physical properties and formation mechanism of spinel iron oxide nanoparticles prepared via the co-precipitation method have been investigated using a multi-technique approach. The obtained magnetic nanoparticles (MNPs) were characterized using the X-ray diffraction, transmission electron microscopy (TEM), SQUID magnetometry, Mössbauer spectroscopy and X-ray absorption near-edge Structure spectroscopy techniques. The synthesis procedure leads to the formation of a spinel structure with an average crystallite size of 9.0(9) nm. The morphology of the particles synthetized under an inert atmosphere was quasi-spherical, while the nanoparticles prepared in air present a faceted shape. The small differences observed in morphological properties are explained by the influence of the reaction atmosphere on the formation mechanism of the MNPs. The magnetic characterization indicates that both samples exhibit superparamagnetic behavior at 300 K. The investigation by means of the Langevin approach at 300 K also leads to equal values for the mean size of the magnetic cores (D_m). Additionally, the analysis of the Mössbauer spectra revealed the lack of spin disorder for both samples, resulting in a high saturation magnetization. The fit of XANES spectrum suggests that about 2/3 of the iron ions reside in a local environment close to that of γ-Fe₂O₃ and about 1/3 close to that of Fe₃O₄ for the sample synthetized in inert atmosphere. Full article

In the present work, ZrO₂-based composites were prepared by adding different amounts of antibacterial magnesium oxide and bioactive and biocompatible hydroxyapatite (HAP) to the inert zirconia. The composites were synthesized by the conventional ceramic processing route and morpho-structurally analyzed by X-ray powder diffraction (XRPD) and scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS). Two metallic dental alloys (i.e., Ni–Cr and Co–Cr) coated with a chitosan (Chit) membrane containing the prepared composites were exposed to aerated artificial saliva solutions of different pHs (i.e., 4.3, 5, 6) and the corrosion resistances were investigated by electrochemical impedance spectroscopy technique. The obtained results using the two investigated metallic dental alloys shown quasi-similar anticorrosive properties, having quasi-similar charge transfer resistance, when coated with different ZrO₂-based composites. This behavior could be explained by the synergetic effect between the diffusion process through the Chit-composite layer and the roughness of the metallic electrode surface. Full article