The layer-by-layer synthesis of LaF₃, ScF₃ nanolayers was perfomed by SILD method. The growth kinetics of mentioned nanolayers was investigated by the ellipsometry method, their composition was explored by FTIR and XP spectroscopy, and the structure was stated by the electron diffraction method. The synthesis of the multilayers mScF₃-nLaF₃, where m and n are the numbers of SILD cycles, was performed in the determined optimal conditions.