The-technology of the liquid phase synthesis of metastable phases in the ZrO 2 -Y 2 O 3 system has been developed. Mesoporous xerogels with the specific surface area of ~350 m 2 /g and monophase nanopow ders (5-10 nm) of the tetragonal solid solution (ZrO 2 ) 0.97 (Y 2 O 3 ) 0.03 have been obtained and their structural peculiarities have been revealed. The efficiency of the suggested technology and good prospects of the syn thesized ZrO 2 based precursors in creating catalysts' substrates have been demonstrated.