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Eingeladener Vortrag
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Highly dispersed vanadium-doped metal oxides such as VOx/ZrO2, VOx/SiO2 and VOx/TiO2/SiO2 with vanadium contents between 0 and 25 mole% were prepared by special bulk preparation methods (coprecipitation and solgel, followed by freeze-drying). Bulk and surface properties of the obtained mixed oxide solid solutions were thoroughly investigated by different analytical methods (Raman and FTIR spectroscopy, TPD, H2-TPR, oxygen isotope measurements etc.). Moreover, the catalytic behaviour of the oxides was studied for the example of the oxidative dehydrogenation (ODH) of propane to propylene. Independent of the preparation method, the catalytic behaviour of vanadium-doped ZrO2 and TiO2 phases is very similar. Both metal oxide solid solutions are very active in propane ODH whereas the catalytic activity of VOx/SiO2 is relatively low. On the other hand, the reduction of the catalytic activity is accompanied by an improved selectivity for the formation of propylene. The correlation between the catalytic activity and the acidity of the oxide systems is discussed. Oxidation experiments with 18O2 clearly show that the ODH reaction occurs according to the Marsvan Krevelen mechanism.
The 57Fe-Moessbauer spectrum of (dmpipzH2)2[FeIII(H2O)2Cl4][FeIII Cl4]Cl2 (1) consists of two doublets caused by a strongly distorted octahedral and a non-distorted tetrahedral component. Both (dmpipzH2)[FeIIIBr4]2 (2) and (trienH2)[FeIIIBr4]Br (3) show only one doublet indicating a more strongly distorted iron(III) species for 2 and a less-distorted one in the case of 3. For all compounds investigated, the ESR spectra reveal the existence of ground states with predominant antiferromagnetic coupling. The Néel temperatures amount to <4.2 K for 1, 4 K for 3 and 48 K for 2. In the case of 2, both the Moessbauer and the ESR spectra reveal the formation of exchange-coupled {FeBr4} units which has been attributed to a significant cation influence. The fine structure of residual paramagnetic [FeBr4]- subunits remaining in the crystalline matrix could be directly determined. Temperature dependent AC and DC susceptibility measurements of 2 and 3 confirmed the results.
Conventional simultaneous thermal analysis, capillary-coupled TGMS, in situ and ex situ Raman and Mössbauer spectroscopy, as well as chemical analysis have been used for the investigation of the first decomposition step of the mixed valence chloroferrate (dmpipzH2)6[Fe(II)Cl4]2[Fe(III)Cl4]2[Fe(II)Cl5][Fe(III)Cl6]. Under argon at ca. 200°C, an almost complete reduction proceeds in a solid state reaction forming Fe(II). It is accompanied by the release of HCl and, to a minor degree, carbon containing species. A multi-phase product with at least two chloroferrate species, coke, and C,H,N-containing polymers is formed. Binuclear iron complexes, such as (dmpipzH)2[Fe(II)2Cl6], and small amounts of (dmpipzH)[Fe(III)Cl4] have been proposed to be the major and minor component of the product mixture, respectively.
A model regarding the generation of acidity in binary metal fluorides has been proposed and its validity has been examined for several binary fluoride systems with the general compositions MF3/M'F3 and MF2/M'F3. In accordance with this hypothesis, the binary systems (CrF3/AlF3, CrF3/FeF3 and AlF3/VF3) do not show acidities larger than the sum of the acidities of the component fluorides. The hypothesis predicts the generation of Lewis acidity when MF2 is the major component (host) and generation of Brønsted acidity when MF3 acts as the host for the MF2/M'F3. The experimental results (surface acidity and catalytic activity) confirmed the predictions made from this hypothesis for binary combinations MgF2/ M'F3 (M'=Cr, Al, Fe, V). The application of this model is discussed in terms of other parameters: ionic radii and the fluoride affinity of the metal fluorides involved.
Powder x-ray diffraction (XRD) defined -Al2O3 has been investigated by x-ray photoelectron spectroscopy (XPS) and x-ray excited Auger electron spectroscopy (XAES). The Au 4f7/2 orbital is used for static charge referencing. This feature originates from well-defined and chemically inert 20 nm highly dispersed gold particles deposited on the sample surface. The particles, with a narrow particle size distribution, were obtained from a highly purified colloidal solution (sodium concentration below 1 mg/l). This procedure allows a determination of gold-referenced XPS and XAES data sets. ©2001 American Vacuum Society.