The invention belongs to the technical field of inorganic materials, and particularly relates to a preparation method of a highly ordered nanoparticle superlattice material. The invention adopts a solution method to prepare monodisperse metal oxide nanocrystalline particles, induces self-assembly of the nanoparticles through solvent evaporation to prepare a three-dimensional ordered nanocrystalline superlattice solid, then carbonizes organic molecules on the surface of the particles at high temperature to obtain a carbon-coated oxide nanoparticle superlattice, removes the metal oxide nanoparticles through acid etching to obtain a highly ordered mesoporous carbon material, uses the mesoporous carbon as a template, injects appropriate precursors into its pore channels, and finally, hydrolyzes, Superlattice materials with corresponding nanoparticles can be obtained by crystallization and other means.

The method disclosed by the invention is simple, the raw materials are easily available, and the cost is low, and the size and shape of the nanoparticles can be controlled by controlling the particle size and shape of the starting metal oxide nanoparticles.