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The transparent titanium-zirconium-containing gel was obtained using heteroligand coordination compounds (namely, alkoxoacetylacetonates) as the precursors. The high-dispersive system “ZrTiO₄ – carbon”, formed after drying of such gel and carbonization of the obtained xerogel, was used to study the evolution of microstructure for the product (ZrTiO₄) during thermal treatment in air for 1 h in the temperature range from 500 °C to 1000°С. It was stated that the formation of crystalline phase occurred in the narrow range 690-730°С. The thermal treatment at 500 °C and 600°С allowed obtaining micro- and mesoporous X-ray amorphous products of the composition ZrTiO₄, with the specific surface area falling in the range 82–150 m²/g. At the higher temperatures the single-phase nanocrystalline powder was prepared (the specific surface area amounted to 2.5–15 m²/g). Particle coarsening took place more …