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Organisationseinheit der BAM
27Al nuclear magnetic resonance spectra of polycrystalline aluminium borate 9Al2O3 · 2B2O3 have been measured in double rotation at 11.7 and 7.0 T and high-speed magic-angle spinning at 7.0, 9.4, 11.7, 14.1 and 17.6 T. Spinning sidebands from the satellite transitions were observed at 7.0 and 14.1 T. Each of the four structural aluminium sites [Al(IV), Al(V)(1), Al(V)(2) and Al(VI)] are observed, characterised and assigned in the spectra. The obtained parameter set gives a fully consistent interpretation in agreement with the crystal structure of the compound.
Humidity-Sensing Materials
(1999)
The structure of glasses in the Li2OB2O3V2O5and ZnOB2O3V2O5systems of a high modifier content ([Li2O, ZnO]/[B2O3] ratio > 1) and 10 to 50 mol % V2O5are investigated by V-KEXAFS and Raman spectroscopy. In the glasses investigated, VO4tetrahedra are the predominant coordination polyhedra for the vanadium ions. The symmetry of the tetrahedra is more or less distorted in comparison with crystalline substances. The VO4tetrahedra can be either directly connected to each other or incorporated into the borate groupings of the BO3and BO4units. An increase in the vanadium content in the glasses reduces the interconnection of structural units and, therefore, the glass transition and crystallization temperatures.
The aluminium oxide films on austenitic steel are prepared from sols of re-dispersed boehmite nano powders in water. After dip-coating of the sol, a heat treatment including drying, calcination and annealing in vacuum at temperatures up to 1100°C is performed to obtain crack-free coatings of a thickness up to 6 µm. XRD measurements detect α- and γ-alumina, a TiOx-phase at the metal/coating interface and a gradient of phase formation in the coating. The strong adhesion on the substrates is due to the layered assembly and gradient composition of the coating caused by an inter-diffusion of metal cations and oxygen in the metal/oxide interface during heat treatment. Residual stress measurements by X-rays result in compressive stresses of 24 GPa in the alumina coatings. The pin-on-disc test shows a remarkable improvement of wear resistance obtained by sol-gel coatings. The α-alumina content and the compressive stress of the coatings correlate with wear resistance of the coatings.
CrN film coatings were prepared by magnetron sputter deposition at different nitrogen partial pressures. The film characterisation by XRD and DTG gives average bulk compositions of Cr2N and CrN for the coatings. Highly sensitive XPS investigations were performed and the chemical and phase compositions of a film surface range of about 10 nm thickness was estimated quantitatively from the deconvoluted peak intensities. It is demonstrated that the composition of the surface of chromium nitride thin films differs from the core and is more complex in constitution. Not only chromium nitrides (Cr2N and CrN) but also chromium oxynitrides and chromium oxides (CrOx and CrOxHy) were detected. Metallic chromium was also found in films prepared at higher nitrogen flow. The concentration of the estimated phases shows dependence on film preparation and additional heat treatment.
A silicon MIS-structure prepared with thin layers of the super-ionic conductor LaF3 and Pd is used to detect hydrogen. The sensor is able to detect hydrogen in a concentration range from below one ppm to the lower flammable limit in air which is 4 vol.-%. The chip operates at room temperature which results in an extremely low energy consumption compared to other hydrogen sensors. Only once per day a short heating pulse is necessary to reactivate the sensor chip. In cooperation with the BAM, a long-term experiment was carried out. The duration of the measurement was about three months, with a hydrogen exposure every two weeks. The sensor signal remained stable over the measured period.