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Eingeladener Vortrag
- nein (51)
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.
EXAFS investigation of an intermediate crystalline phase in TiO2-rich strontium borate glasses
(1995)
Glasses in the systems Li2OB2O3V2O5 and ZnOB2O3V2O5 as well as crystalline reference substances were investigated by V-K-EXAFS. The glasses have a high modifier content ([Li2O, ZnO]/[B2O3] ratio>1) and contain 1050 mol% V2O5. The VO interatomic distance, coordination number and DebyeWaller factor were determined from the analysis of the measured absorption spectra. In the glasses investigated (and in binary lithium or zinc vanadate glasses too) VO4 tetrahedra are the predominant coordination polyhedra for the vanadium ions. The symmetry of the tetrahedra is more or less distorted in comparison to crystalline substances. The VO4 tetrahedra can be either directly connected to each other or incorporated into borate BO3/BO4 groupings. Structural elements which are comparable to those in crystalline substances can be discussed. In glasses of the metaborate composition, vanadium can be incorporated in chain or ring [BØ2O-]n metaborate groupings. With increasing V2O5 content the vanadium ions can extensively replace boron ions and form distorted tetrahedra in VØ2O2- metavanadate groups. In glasses of high modifier content and low vanadium amount the vanadium ions create nearly regular tetrahedra of isolated VO43- ortho- or V2ØO64- pyrovanadate groups in the presence of B2ØO44- pyroborate, BO33- orthoborate and BØ4- groups.
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 paper demonstrates the scope of the differential thermal analysis coupled with the thermal gravimetry as an express method for estimation of thin film protecting ability and oxidation kinetics. Oxidation of an iron foil protected by the PVD titanium nitride thin film coating was investigated as well as non-isothermal oxidation of PVD thin films of TiN (two types of the preparation procedure), (Ti,Nb)N and (Ti,Al)N isolated from a substrate by dissolving them in an acid. Additions of aluminium and niobium are expected to improve chemical, thermal and biomedical properties of thin films for their technical application. It was established that the addition of niobium decreases, whereas the addition of aluminium not only increases the thermal stability of TiN coatings, but also changes the oxidation mechanism. It was demonstrated that the TiN film oxidation is a many-staged process depending on the heating rate. An opportunity of a quite formal treatment for getting Kissinger's estimation of kinetics parameters of different oxidation stages is also demonstrated.
Es wurden Gläser im System Li2O-B2O3-V2O5 und ZnO-B2O3-V2O5 wie auch kristalline Referenzmaterialien mit Hilfe der Röntgenabsorptions- (V-K-EXAFS, -XANES) und der RAMAN-Spektroskopie untersucht. Zur Diskussion der Ergebnisse wird angenommen, dass in den Gläsern in Abhängigkeit von der chemischen Zusammensetzung diskrete Sauerstoffkoordinationspolyeder der Kationen in unterschiedlicher Verknüpfung vorliegen.
1. Die Gläser enthalten vor allem BO3- bzw. BO4- sowie VO4-Polyeder.
2. Die VO4-Tetraeder besitzen abhängig von der Glaszusammensetzung eine unterschiedliche Verzerrung. Sie verknüpfen sich zu Struktureinheiten ähnlich denen der kristallinen Vanadate oder sie werden in Boratstrukturen eingebaut.
3. In Gläsern mit einem hohen Netzwerkwandler-Gehalt und geringer Vanadiumoxid-Konzentration treten reguläre Tetraeder von isolierten Ortho- oder Pyrovanadat-Gruppen in Gegenwart von Pyroborat-, Orthoborat- und BO4-Gruppen auf. Mit steigendem V2O5-Gehalt werden zunehmend verzerrte Tetraeder gebildet, die sich z. B. zu Metavanadat-Gruppen verknüpfen oder in Metaborat-Baugruppen eingebaut werden.