Thermal decomposition of zirconyl oxalate hydrate was studied using DTA, TG, QMS and XRD techniques. It was shown that decomposition occurs in two stages: dehydration to anhydrous oxalate and next, decomposition to zircon oxide (zirconia). These steps are not well separated. We observed that significant amount of water are released during second stage of decomposition. Zircon dioxide is obtained in tetragonal form. Moreover, we consider some dependences between conditions of preparations zirconyl oxalate hydrate and some properties of solid product of its decomposition. Although the reaction of thermal decomposition of zirconyl salts is generally utilized in technology, many aspects of this process are still not sufficiently explained. In our work, we present some new interesting observations concerning thermal behaviour of zirconyl oxalate.