Fourier Transform Raman spectroscopy of gels derived from modified Tetra(-n-butoxy)zirconium (IV)

Computer Science

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Gels And Sols, Organic Compounds, Polymers

Scientific paper

Reaction products of alkoxides with certain modifying agents and the determination of the structure of zirconia sols and gels can be observed through the use of vibrational spectroscopy. FT-Raman spectroscopy has proved to be a useful technique in observing the gelation process and the resulting structure. Raman spectroscopy has been used to follow the structural evolution of the gel from the mixing the two solvents to the final stages of gelation. The unmodified gel spectra consist of strong bands at 1049 and ~260 cm-1 which are assigned to the aquated nitrate N-O symmetric stretch and to the Zr-O symmetric stretch respectively. These bands are also present in the acetic and propanoic modified sols and gels, produced by the peptisation of the hydrolysate using nitric acid as the stabilizing agent. The spectra of the acetate and propanoate systems exhibit additional strong peaks at 535, 1350, 1425, 1450, and 1560 cm-1. The latter three bands are assigned to the co-ordinated acetate and propanoate. The band positions indicate that both monodentate and bridging ligands are present within the gel. The spectra of the hydrolysate has a less complex carboxylate region indicating only one type of ligand present. The absence of Zr-O-C bands between 1200 and 1000 cm-1 indicate that there is no residual alkoxide present within the gel.

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