A two-phase spherical Y 2 O 3 /ZnO nanocomposite particle with a diameter variable in the series of 70, 130, 180, 250, and 400 nm (variance ≤15%) has been obtained; the first phase is a mesoporous Y 2 O 3 matrix, while the second is a crystalline ZnО phase located in the size-limited pore volume. Specific features of ZnO nanocrystals formed on the high-curvature surface of pores with excess surface energy are studied. It is shown that the thermally activated coarsening of ZnO crystallites accompanied by an increase in the nanophase structural quality occurs during Y 2 O 3 /ZnO annealing in the temperature range t = 600-800°C. It is established that the wurtzite lattice is strained on the surfaces of small Y 2 O 3 pores.