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'C. It was stated that the formation of crystalline phase occurred in the narrow range 690-730 degrees C. The thermal treatment at 500 degrees C and 600 degrees C allowed obtaining micro- and mesoporous X-ray amorphous products of the composition ZrTiO4, with the specific surface area falling in the range 82-150 m(2)/g. At the higher temperatures the single-phase nanocrystalline powder was prepared (the specific surface area amounted to 2.5-15 m(2)/g). Particle coarsening took place more extensively at temperatures >= 700 degrees C was shown. For the ZrTiO4 nanopowder crystallized under the mildest conditions at the temperature of 700 degrees C, chemoresistive gas-sensitive properties were studied for the first time. The material showed a high reproducible response at 1-20% O-2 and 200-10,000 ppm H-2 at a relatively low detection operating temperature of 450 degrees C.