The Fe 3 O 4 @HxMoO 4 ·nH 2 O nanolayers were synthesized on the solid surface for the first time by Successive Ionic Layer Deposition (SILD) method with using an aqueous Fe 3 O 4 suspensions and (NH 4 ) 2 MoO 4 solutions. The obtained nanolayers were investigated by XRD, SEM, EDX, FTIR spectroscopy and magnetization measurement techniques. SEM images showed that the nanolayers formed by nanoparticles of size approximately 15-20 nm. The synthesized nanolayers exhibited superparamagnetic properties with the saturation magnetization value of 55 emu/g.