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The structure and morphology of monodisperse spherical particles of (YEu)O solid solutions prepared through the low-temperature thermolysis of an amorphous precursor under isothermal conditions ( t = 800°C) have been analyzed in detail in relation to the particle size and composition. The results demonstrate that, in addition to having a polycrystalline (block) structure, the spherical (YEu)O particles are porous, with a mesoscopic residual pore size. Reducing the diameter of the spherical particles from 400 to 70 nm reduces their porosity and improves their structural perfection. The addition of Eu cations stimulates the growth of crystalline blocks that form a spherical particle, activating diffusion processes in the cation sublattice of the solid solution. [ABSTRACT FROM AUTHOR]