Environmental study of miniature slip rings

Investigation studied the long term operation of miniature slip ring assembles in high vacuum of space and included the influence of ring, brush, and insulator materials on electrical noise and mechanical wear. Results show that soft metal vapor plating and niobium diselenide miniature slip rings are beneficial

The influence of chemical transport via vapour phase on the properties of chloride and caesium doped V-Fe mixed oxide catalysts in the oxidation of butadiene to furan

Chloride and caesium doped V-Fe mixed oxides prepared by different methods and calcined under vapour-phase transport-restricted conditions showed a high initial furan yield of up to 40 mol-% in the oxidation of butadiene. However,after only a few hours on stream a significant loss of activity and selectivity was observed. The reason for this undesirable property was investigated using different bulk and surface-sensitive characterisation methods such as x-ray diffraction, x-ray photoelectron spectroscopy, ransmission electron microscopy and chemical methods. The data obtained for the structure, morphology, and composition of the fresh and used catalysts were correlated with their activity and selectivity properties. The presence of chloride ions was found to be surprisingly necessary for the origin of furan selectivity even up to 50 %, which was however stable only for a short period of time. Chemical transport via chlorides or bromides was observed to be essential for the formation as well as the maintenance of the activity and selectivity properties of the system. The results obtained are interpreted with an assumption that the formation of volatile halides is necessary to form disperse VOx species, which act as active and selective centres for the present reaction. Models for the formation and deactivation of these centres are discussed in this work. In addition, the possible roles of caesium and iron oxides in the catalytic system are also described and disputed

A new test specimen for the determination of the field of view of small-area X-ray photoelectron spectrometers

Small-area/spot photoelectron spectroscopy (SAXPS) is a powerful tool for the investigation of small surface features like microstructures of electronic devices, sensors or other functional surfaces, and so forth. For evaluating the quality of such microstructures, it is often crucial to know whether a small signal in a spectrum is an unwanted contamination of the field of view (FoV), defined by the instrument settings, or it originated from outside. To address this issue, the d80/20 parameter of a line scan across a chemical edge is often used. However, the typical d80/20 parameter does not give information on contributions from the long tails of the X-ray beam intensity distribution or the electron-optical system as defined by apertures. In the VAMAS TWA2 A22 project “Applying planar, patterned, multi-metallic samples to assess the impact of analysis area in surface-chemical analysis,” new test specimen was developed and tested. The here presented testing material consists of a silicon wafer substrate with an Au-film and embedded Cr circular and square spots with decreasing dimensions from 200 μm down to 5 μm. The spot sizes are traceable to the length unit due to size measurements with a metrological SEM. For the evaluation of the FoV, we determined the Au4f intensities measured with the center of the FoV aligned with the center of the spot and normalized to the Au4f intensity determined on the Au-film. With this test specimen, it was possible to characterize, as an example, the FoV of a Kratos AXIS Ultra DLD XPS instrument

Co-based heterogeneous catalysts from well-defined Α-diimine complexes : Discussing the role of nitrogen

Ar-BIANs and related \uce\ub1-diimine Co complexes were wet impregnated onto Vulcan\uc2\uae XC 72 R carbon black powder and used as precursors for the synthesis of heterogeneous supported nanoscale catalysts by pyrolysis under argon at 800\uc2\ua0\uc2\ub0C. The catalytic materials feature a core-shell structure composed of metallic Co and Co oxides decorated with nitrogen-doped graphitic layers (NGr). These catalysts display high activity in the liquid phase hydrogenation of aromatic nitro compounds (110\uc2\ua0\uc2\ub0C, 50 bar H2) to give chemoselectively substituted aryl amines. The catalytic activity is closely related to the amount and type of nitrogen atoms in the final catalytic material, which suggests a heterolytic activation of dihydrogen

Identifying the location of Cu ions in nanostructured SAPO 5 molecular sieves and its impact on the redox properties

Combining X ray Absorption Fine Spectroscopy XAFS with Anomalous Small Angle X ray Scattering ASAXS determines the location of Cu2 ions in silicoaluminophosphate SAPO 5 frameworks prepared by hydrothermal crystallization or impregnation. As expected, for the hydrothermally prepared sample, incorporation in the SAPO 5 framework was observed. For the first time preferential location of Cu2 ions at the inner and outer surfaces of the framework is determined. Temperature Programmed Reduction TPR and X ray Photoelectron Spectroscopy XPS investigations demonstrated that such Cu2 is stable in an argon Ar atmosphere up to 550 C and can only be reduced under a hydrogen atmosphere. In contrast, Cu2 deposited by impregnation on the pure SAPO 5 framework can be easily reduced to Cu in an Ar atmosphere. At lower Cu amounts, mononuclear tetrahedrally coordinated Cu species were formed which are relatively stable in the monovalent form. In contrast, at higher Cu amounts, CuO particles were found which change easily between the mono and bivalent specie

Assessing Optical and Electrical Properties of Highly Active IrO_x Catalysts for the Electrochemical Oxygen Evolution Reaction via Spectroscopic Ellipsometry

Efficient water electrolysis requires highly active electrodes. The activity of corresponding catalytic coatings strongly depends on material properties such as film thickness, crystallinity, electrical conductivity, and chemical surface speciation. Measuring these properties with high accuracy in vacuum-free and non-destructive methods facilitates the elucidation of structure–activity relationships in realistic environments. Here, we report a novel approach to analyze the optical and electrical properties of highly active oxygen evolution reaction (OER) catalysts via spectroscopic ellipsometry (SE). Using a series of differently calcined, mesoporous, templated iridium oxide films as an example, we assess the film thickness, porosity, electrical resistivity, electron concentration, electron mobility, and interband and intraband transition energies by modeling of the optical spectra. Independently performed analyses using scanning electron microscopy, energy-dispersive X-ray spectroscopy, ellipsometric porosimetry, X-ray reflectometry, and absorption spectroscopy indicate a high accuracy of the deduced material properties. A comparison of the derived analytical data from SE, resonant photoemission spectroscopy, X-ray absorption spectroscopy, and X-ray photoelectron spectroscopy with activity measurements of the OER suggests that the intrinsic activity of iridium oxides scales with a shift of the Ir 5d t2g sub-level and an increase of p–d interband transition energies caused by a transition of μ1-OH to μ3-O species

111 oriented gold nanoplatelets on multilayer graphene as visible light photocatalyst for overall water splitting

[EN] Development of renewable fuels from solar light appears as one of the main current challenges in energy science. A plethora of photocatalysts have been investigated to obtain hydrogen and oxygen from water and solar light in the last decades. However, the photon-to-hydrogen molecule conversion is still far from allowing real implementation of solar fuels. Here we show that 111 facet-oriented gold nanoplatelets on multilayer graphene films deposited on quartz is a highly active photocatalyst for simulated sunlight overall water splitting into hydrogen and oxygen in the absence of sacrificial electron donors, achieving hydrogen production rate of 1.2 molH2 per gcomposite per h. This photocatalytic activity arises from the gold preferential orientation and the strong gold–graphene interaction occurring in the composite system.Financial support by the Spanish Ministry of Economy and Competitiveness (Severo Ochoa and CTQ2012-32315) and Generalitat Valenciana (Prometeo 2013-019) is gratefully acknowledged. D.M. and I.E.-A. thank to Spanish Ministry of Science for PhD scholarships.Mateo Mateo, D.; Esteve Adell, I.; Albero Sancho, J.; Sánchez Royo, JF.; Primo Arnau, AM.; García Gómez, H. (2016). 111 oriented gold nanoplatelets on multilayer graphene as visible light photocatalyst for overall water splitting. Nature Communications. 2016(7):1-8. https://doi.org/10.1038/ncomms11819S1820167Lv, X. J., Zhou, S., Huang, X., Wang, C. & Fu, W. F. Photocatalytic overall water splitting promoted by SnOx-NiGa2O4 photocatalysts. Appl. Cat. B: Environ. 182, 220–228 (2016).Xu, J., Wang, L. & Cao, X. 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