The wide application of electromagnetic technology has led to increasingly frequent information transmission and communication interconnection. When the intensity of the disordered radiation of electromagnetic waves is too high, it will cause electromagnetic pollution and pose a huge threat to human health or the survival of other animals and plants. How to ingeniously design absorbing materials is the key to solving the problem. This paper proposes a new design concept. The Co-based zeolite imidazolite-structured material ZIF-67 was selected as the main body of the metal-organic frameworks (MOFs) template, and the dodecahedral structured ZIF-67 nanoparticles were prepared using the classic ion-ligand process. Subsequently, a dodecahedral NiCo-LDH nanoparticle precursor composed of NiCo bimetallic hydroxide nanosheets with hollow edges and interior was obtained based on the liquid-phase cationic etching process. On this basis, thioacetamide (TAA) was selected as the vulcanizing agent, and the ZIF-67-derived sulfide inheriting the micro-nano structure of the precursor was obtained through liquid-phase hydrothermal vulcanization. The vulcanization growth mechanism and electromagnetic wave absorption mechanism of the MOF_S-derived sulfide were deeply explored.