Abstract: The invention relates to a method of preparation of lamellar porous microstructures and nanostructures of various density based on controlled vacuum freeze-drying of a liquid dispersion of nanoparticles. The liquid dispersion of particles is rapidly freezed into solid state inside a tightly closed volume. In this form it is submitted to vacuum freeze-drying with required rate of sublimation of molecules of a liquid dispersion medium, until their total removal, accompanied by the creation of lamellar microstructures and nanostructures. The orientation of the normal vector of the dominant surface of sublimation interface can be set with regard to the required properties of the final sublimate structure from vertically upwards to vertically downwards. The sublimation rate is adjusted by combination of vacuum depth and external heating of the sublimation interface of the frozen material.