Xerogels and powders of Al2O3–ZrO2–CeO2 systems with different pore structure and matrixes of ZrO2 and Al2O3 are obtained. The specific surface area of xerogels with ZrO2 matrix and Al2O3 matrix exceeds 200 and 90 m2/g, respectively. After calcinations at 950°C, the powders retain nanoscale, with the size of individual particles ranging from 70 to 28 nm. The main crystalline phase in these powders is a solid solution of tetragonal zirconia. Total ethanol conversion of xerogels with ZrO2 and Al2O3 matrixes has similar values. Selectivity to ethylene conversion is about 50% and does not depend on calcination temperature. For samples with an Al2O3 matrix, ethylene selectivity of 50% was reached after heating at 950°C. It is shown that the catalytic activity of ethanol conversion reaction is higher for samples with a more crystallized phase based on solid solution of tetragonal zirconia, namely, for samples with the ZrO2 matrix calcined at 950°C. © 2018, Pleiades Publishing, Ltd.