Novel sol-gel prepared zinc fluoride: synthesis, characterisation and acid-base sites analysis

The fluorolytic sol-gel route sets a milestone in the development of synthesis methods for nanoscopic fluoride materials. They exhibit fundamentally distinct properties in comparison to classically prepared metal fluorides. To broaden this area, we report in this paper the first fluorolytic sol-gel synthesis of ZnF₂. The obtained sol was studied with dynamic light scattering (DLS). The dried ZnF₂ xerogel was investigated with elemental analysis, thermal analysis, powder X-ray diffraction (XRD), solid-state MAS NMR, and N₂ adsorption-desorption measurements. The characterisations revealed a remarkably high surface area of the sol-gel prepared ZnF₂. To determine key parameters deciding its prospects in future catalytic applications, we studied the surface acidity-basicity by using in situ FTIR with different probe molecules. Compared to the previously established MgF₂, weaker Lewis acid sites are predominant on the surface of ZnF2 with some base sites, indicating its potential as a heterogeneous catalyst component. In short, we believe that the successful synthesis and detailed characterisation of nanoscopic ZnF₂ allow follow-up work exploring its applications, and will lead to studies of more metal fluorides with similar methods

Edelmetallbeladene Aluminiumhydroxidfluoride als neue heterogene Katalysatoren

Hauptaufgabe dieser Promotionsarbeit war es, eine neue Sol-Gel basierte Syntheseroute zur Darstellung edelmetallbeladener (Pd, Pt, Ag und Au) Aluminiumhydroxidfluoride zu entwickeln. Derartige Katalysatoren besitzen sowohl Lewis- als auch Brønsted-saure, sowie hydrogenierungsaktive Zentren. Solche multifunktionellen Katalysatoren können für mehrstufige Umsetzungen von Substraten in Eintopfverfahren eingesetzt werden. Das Potential der dargestellten Katalysatoren wurde in der zweistufigen Umsetzung von Citronellal zu Mentholen und der dreistufigen Reaktion von Citral zu Mentholen gezeigt.The main aim of this thesis was to develop a new sol gel based synthesis route to noble metal loaded (Pd, Pt, Ag and Au) aluminium hydroxide fluorides. These catalysts provide Lewis as well as Brønsted acidity and hydrogenation ability. Those multifunctional catalysts can be used for multi step conversions of substrates performed in a one pot process. The potential of the synthesized catalysts was shown in the two step conversion of citronellal to menthols and in the three step conversion of citral to menthols

Encapsulation of ZnO particles by metal fluorides: Towards an application as transparent insulating coatings for windows

Because ZnO is a promising candidate for getting efficient films or varnishes with thermal insulating abilities for windows applications, the effect of the encapsulation of ZnO particles in shells of low refractive index material on the improvement of the visible light transmission was investigated. ZnO-MgF2 core-shell particles were synthesized by deposition of fluoride sols on ZnO particles through a vacuum slip casting process like. The transmission behaviours were first indirectly studied by diffuse reflexion measurements on powder beds. Then, particle films were elaborated by a screen printing process which ensured direct transmission measurements. The encapsulation of ZnO particles with a coating shell of 1.3 wt.% of MgF2 improves the visible light transmission of 32%