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Organisationseinheit der BAM
Aluminas with Fe2O3 particles finely divided in the Al2O3 matrix were prepared via a crystalline precursor derived from ammonium dawsonite and its calcination. The precursors with Fe content between 1 and 10 wt% were synthesized by reaction of ammonium hydrogen carbonate with mixtures containing aluminium ammonium sulfate and ferric ammonium sulfate. The characterization of the as-synthesized and calcined products by chemical analysis, XRD, EPR, Mössbauer, TEM and adsorption measurements shows that all the Fe3+ ions are incorporated into the structure of dawsonite when the Fe content is low and that the calcined materials with micropores and mesopores (maximum 3040 Å) also contain very small Fe2O3 particles (<10 nm) at higher Fe contents.
Nanocrystalline particles of high temperature pretreated titania, zirconia or hafnium oxide, embedded in a carbon matrix, have been found to catalyze the aromatization of n-octane into ethylbenzene (EB) and o-xylene (OX) with high selectivity. The carbon matrix itself is catalytically not active, but seems to co-operate with the transition metal oxides in such a way that the various metal oxide/carbon composite materials exhibit equal selectivity patterns. In detail, the carbon component stabilizes a high dispersion of the oxides during the high temperature pretreatment procedure. This thermal treatment results in a destruction of surface acidity of the oxides, which would otherwise be responsible for undesirable consecutive and parallel reactions. Moreover, the carbon component is involved in the deep dehydrogenation of alkanes to multiple unsaturated alkenes. This is explained by the ability of surface carbon atoms to interact with hydrogen. The bulk and surface structure of the catalysts have been characterized by XRD, specific surface area measurements, XPS, UPS, Raman spectroscopy, in situ ESR and DRIFT spectroscopy.
The slip-rolling resistances of hard and stiff thin films under high Hertzian contact pressures can be improved by optimizing the 'coating/substrate systems'. It is known from former investigations that the so-called 'egg-shell' effect is no general hindrance for high slip-rolling resistance of thin hard coatings. The coating stability depends more on specific deposition process and coating/substrate interface design. In this article it is experimentally shown, that pure amorphous carbon thin films with hardness between 15 and 63 GPa can be slip-rolling resistant several million load cycles under a maximum Hertzian contact pressures of up to 3.0 GPa. Whereas all coatings were stable up to 10 million load cycles in paraffin oil at room temperature, reduced coating lifetime was found in SAE 0W-30 engine oil at 120°C. It was shown how the coating hardness and the initial coating surface roughness influence the running-in process and coating lifetime. No clear correlation between coating hardness and coating lifetime could be observed, but friction coefficients seem to be reduced with higher coating hardness. Very low friction down to ~0.03 in unmodified engine oils was found for the hardest ta-C film.------------------------------------------------------------------------------------------------------------------------------------------------
Die Wälzbeständigkeit von harten und steifen Dünnschichten unter hohen Hertzschen Kontaktpressungen kann durch die Optimierung des 'Beschichtung/Substrat Systems' deutlich verbessert werden. Aus vorangegangenen Untersuchungen ist bekannt, dass der so genannte 'Eierschaleneffekt' kein generelles Hindernis für eine hohe Wälzbeständigkeit für harte Dünnschichten darstellen muss. Die Stabilität der Beschichtungen hängt vielmehr von dem spezifischen Prozessparametern und dem Schicht/Substrat Grenzflächendesign ab. In diesem Artikel wird experimentell nachgewiesen, dass reine amorphe Kohlenstoffdünnschichten mit Härtewerten zwischen 15 und 63 GPa für mehrere Millionen Lastzyklen unter maximalen Hertzschen Kontaktpressungen bis 3.0 GPa überrollbeständig sein können. Während alle Beschichtungen bis 10 Millionen Lastzyklen in Paraffinöl bei Raumtemperatur keine Defekte aufweisen wurde unter Verwendung eines SAE 0W-30 Motorenöls bei 120°C eine Verringerung der Überrollbeständigkeit nachgewiesen. Es wurde nachgewiesen, wie die Schichthärte und ursprüngliche Oberflächenrauheit der Beschichtung den Einlaufprozess und die Lebensdauer beeinflussen. Es konnte keine offensichtliche Korrelation zwischen Schichthärte und Lebensdauer festgestellt werden, allerdings wurde eine scheinbare Reduktion des Reibwertes mit steigender Schichthärte beobachtet werden. Dabei zeigte die härteste ta-C Schicht unter Verwendung des Motorenöls sehr geringe Reibwerte mit ~0.03.
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.
Wälzbeständigkeit von ta-C Dünnschichten unter hohen Hertzschen Beanspruchungen bis zu 3000 MPa
(2010)
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.
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.
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.