In this paper, we present the experimental results on the application of the pulsed laser deposition (PLD) method to form functional SiO2 and MgO layers in contact with Fe3Si and Fe ferromagnetic electrodes In situ X-ray photoelectron spectroscopy and low-energy ion scattering spectroscopy, in situ conversion electron Mössbauer spectroscopy and Rutherford backscattering and channeling of light ions were used to study the structural properties and morphology of formed ultrathin SiO2 and MgO layers, as well as the chemical and phase composition of Fe3 Si/SiO2 and Fe/MgO interfaces.