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EXAFS investigation of an intermediate crystalline phase in TiO2-rich strontium borate glasses
(1995)
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.
A comprehensive analysis of composition and structure is essential for the development of new materials with tailored properties. We will demonstrate the application of SEM, XPS and XRD for the development of thin films containing nano-scaled electrical conductive particles for application in hybrid resistors.
The films were prepared using the sol-gel process and precursor solutions were synthesized from an acid hydrolysis of a mixture of TEOS, water and ethanol. Alcoholic solutions of ruthenium chloride were then allocated to obtain up to 30 vol% filler in the films. The films were precipitated by dip-coating on silicon, silica or glass sheets and heat treated at up to 600°C in air or nitrogen atmospheres.
A nano-structured morphology could be identified consisting of homogeneously dispersed crystalline RuO2 particles of 10 to 180 nm in size, in an amorphous SiO2 matrix. Film morphology can be varied using the synthesis process. The resistivity of the films was measured by an I-V measurement system. It changes drastically from 109·cm to 10-2·cm according to the amount of dispersed conductive particles.
The results show that composition-structure-property relations can be described by use of sophisticated analytical methods.
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.