EFFECTS OF ZRO2 PRECURSORS ON THE SYNTHESIS OF V-ZRSIO4 SOLID-SOLUTIONS BY THE SOL-GEL METHOD

The preparation of V-ZrSiO4 solid solutions starting from different ZrO2 precursors by using sol-gel methods is reported. The starting materials were hydrolysed and the dried gels were fired at a temperature between 500 and 900-degrees-C with soaking times of 12 h. The organic character of zirconia precursors was stronger, i.e. the starting material had more carbon atoms, a higher temperature was necessary to make the first crystalline phase appear (ZrO2(tetragonal)) and the temperature range for the whole phase transformation was narrower. In all dried gel samples the presence of infrared bands which might be associated with either Si-O-Zr or Si-O-V was not observed. On the other hand, some bands could be attributed to a silica network and ZrO8 groups. The main steps in V-ZrSiO4 solid solutions were confirmed. ZrO2(tetragonal) is crystallized on heating from an amorphous sample. The ZrO2(tetragonal) --> ZrO2(monoclinic) phase transformation then occurs and immediately afterwards the zircon formation begins. Finer textures in samples were obtained from polymeric gels rather than for colloidal gel samples, as seen from the scanning electron micrographs.