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Organisationseinheit der BAM
α(1 0 0) Dislocations are observed in nickel-base superalloys after creep deformation at high temperatures and low stresses. They are formed in the γ/γ´ interfaces by a three step mechanism. First, primary dislocations with Burgers vector α/2(1 0 1) and 60° character are left behind in the interfaces when dislocation loops glide through the γ channels. The 60° dislocations move into edge orientation and react forming secondary dislocations α/2(1 1 0). In the third step, new primary dislocations are knit into the already existing meshes of primary and secondary dislocations, which results in hexagonal misfit dislocation networks consisting of secondary dislocations α/2(1 1 0) and tertiary dislocations α(1 0 0), both of edge type. This self-organisation process is explained by dislocation theory and crystallography.
Creep deformation accelerates when the α(1 0 0) interfacial dislocations enter the γ´ phase. During their climb towards the opposite interface, they attain a characteristic rectangular shape. This shape and the importance of the α(1 0 0) super dislocations for creep deformation are discussed.
Iron-based catalysts are employed in CO2-FTS due to their ability to convert CO2 into CO in a first step and their selectivity towards higher hydrocarbons in a second CO hydrogenation step. According to the literature, iron carbides represent the active phase for hydrocarbon formation and are claimed to emerge in the presence of CO. We propose nanostructured FeOx films as model systems to assess information about the complex phase transformations during CO2-FTS. Mesoporous hematite, ferrihydrite, maghemite, maghemite/magnetite films were exposed to CO2-FTS atmospheres at 20 bar and 300°C. Up to three distinct phases were observed depending on the timeon-stream (TOS): a sintered maghemite/magnetite phase, a carbidic core-shell structure, and a low-crystalline, needle-type oxide phase. Our findings indicate that the formation of an intermediary maghemite/magnetite phase, predominant after short TOS (30 h), precedes the evolution of the carbide phase.
Yet, even after prolonged TOS (185 h), no full conversion into a bulk carbide is observed.
As a model for spray drying the early stages of crystallization of complex molybdate catalyst precursors were monitored online in droplets levitated acoustically. Synchron X-ray scattering techniques were applied to study the drying process of a typical molybdate catalysts precursor prepared from Ni-,Fe-,Bi-nitrate, ammonium heptamolybdate and H3PO4. Comparison with diffraction patterns obtained from sessile droplets shows significant differences in the crystal growth, whereas the final crystal structure – including a Keggin-type anion – is identical in both cases. The levitated samples exhibit a decelerated growth with a large number of small crystallites at the beginning of the crystallization, whereas in case of the sessile droplets a small number of large crystallites were observed after a few minutes. The acoustic levitation using an ultrasonic trap proves to be an elegant tool to mimic spray drying and offers new possibilities in relation to the understanding of the drying process.
The tribological behaviour of MoS2/ta-C double layer coatings deposited by Laser-Arc technology was investigated in vacuum and air. In vacuum environment, the friction coefficient against steel balls varies between 0.005 and 0.02 depending on the contact pressure. At high contact pressures, the friction coefficient is as low as 0.005 and the life time between 340,000 and 500,000 cycles. Furthermore, it is shown that a ta-C base layer improves the performance of MoS2 coating.
Surface analyses were performed before and after the tribological tests by means of SEM, EDX, XRD, and TEM. They show that in the top layer beneath the sliding surface crystallization of the initially quasi-amorphous MoS2 took place. TEM images also verified an orientation of the basal MoS2-lattice planes parallel to the surface.
Monometallic Cu and bimetallic Cu/Au-TiO2 catalysts were prepared by impregnation (IM) and reductive precipitation (RP)methods in sequential (SP) and simultaneous mode (CP) and tested for photocatalytic H2 generation from H2O/Methanol mixtures with visible (400–700 nm) and UV/Vis light (320– 500 nm). Comprehensive studies by high-resolution (HR)-STEM, X-ray photoelectron spectroscopy (XPS), and different in situ methods (X-ray Absorption near-edge structure (XANES), UV/Vis, and EPR spectroscopy) revealed that IM leads to dispersed surface Cu species with no clear particle formation, which is poorly active under visible light, whereas plasmonic Cu0 nanoparticles formed by RP are about three times more active under the same conditions. In Cu/Au-TiO2 catalysts prepared by RP-SP, highly dispersed Cu surface species boost H2 production under UV/Vis light, owing to the effective separation within TiO2 and electron trapping by Cu, whereas small Cu0 and Au0 particles remain widely separated. When Cu/Au-TiO2 catalysts are prepared by RP-CP, mixed Cu/Au particles of uniform size (4–8 nm) provide the highest H2 evolution rates under visible light, owing to effective surface plasmon resonance absorption.
Influence of Sb on the structure and performance of Pd-based catalysts: An X-ray spectroscopic study
(2017)
Combined X-ray photoelectron and absorption fine spectroscopy (XAFS) investigations on 10 wt % Pd–16 wt % Sb/TiO2 catalyst allow new insight into the impact of the co-component Sb on the active Pd species, which catalyzes the gas-phase acetoxylation of toluene to benzyl acetate. Ex situ Pd 3d XPS and Pd L-edge XANES studies indicate the presence of an excess electron charge on metallic Pd species (more 4d electrons than in Pd metal) formed after several hours of stream. This observation was explained by the electron transfer from metallic Sb incorporated into the Pd bulk to the neighboring Pd atoms. TEM-EDX analysis confirms the presence of intermixed Pd–Sb particles with an atomic ratio of between 5 and 6 in the most active catalysts and of 3 in deactivated samples. In situ Sb-K-edge XAFS investigations provide evidence that the Pd–Sb interaction is more pronounced under reaction feed than in the ex situ samples.
A new setup is presented which enables simultaneous wide- and small-angle X-ray scattering (WAXS/SAXS) and Raman spectroscopic experiments during the synthesis of Mo-based mixed oxide catalyst precursors at the µ-spot beamline at the Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung (BESSY). Furthermore, we report about the separate monitoring of the same reactions under comparable conditions by simultaneous combined ATR/UVvis/Raman spectroscopic measurements. For testing the performance of both experimental setups two syntheses were described comprising the precipitation of metal molybdates by mixing solutions of metal nitrates and ammonium heptamolybdate. Additionally, the effect of H3PO4 admixture on precipitation was investigated. The combined evaluation of spectroscopic and WAXS/SAXS data allows the discrimination between different molybdate species appearing in solution and precipitate. Furthermore, these molybdate species could be assigned to separate phases of different crystallinity.
Moiré fringes for misfit measurements at incoherent y/y'-interfaces of nickel-base superalloys
(1998)
Mittels lasergesteuerter gepulster Vakuumbogentechnologie (Laser-Arc) wurde eine reihe von reinen MoS2-Schichten sowie Kombinationsschichten aus MoS2 und tetraedrischem amorphen Kohlenstoff (ta-C) hergestellt. Mit diesen Schichtvarianten erfolgten tribologische Tests im Vakuum sowie in Atmosphäre. Dabei wurden im Hochvakuum reibungskoeffizienten bis zu 0,005 gemessen. Durch die Verwendung einer ta-C unterschicht konnte eine Lebensdauer von über 5×105 Lastzyklen erreicht werden. Zudem erwies sich diese unterschicht als vorteilhaft für das tribologische Verhalten der MoS2/ta-C Schichten unter atmosphärischen Bedingungen. -------------------------------------------------------------------------------------------------------------------------------------------
A series of MoS2 and combined MoS2/ta-C coatings were prepared by lasercontrolled arc evaporation (Laser-Arc) in order to study the tribological coating behaviour under vacuum and atmospheric conditions. Very low friction coefficients down to 0.005 were measured under high vacuum. By using a ta-C underlayer beneath the MoS2 a increased lifetime up to 5×105 load cycles could be obtained. Also under atmospheric conditions the underlayer had a beneficial effect on coating performance.
A new experimental technique (repeated load annealing of flat wedge shaped specimens) was proposed for characterization of microstructural degradation under creep conditions. This technique was applied to investigate the microstructural degradation of the nickel-base superalloy CMSX-4 in a wide range of temperatures and stress levels. The results obtained allowed to describe analytically the kinetics of rafting, which is important to predict the reduction of fatigue lifetime and yield stress.