Isolation structure has been proven to be an effective method for constructing electromagnetic shielding composites, achieving high electrical conductivity with shallow filler content and high-efficiency electromagnetic shielding. However, there are still many challenges in further optimizing the design and improving absorption. This article designed a hybrid isolation structure using nylon magnetic microspheres and polystyrene (PS). First, we prepared PA magnetic microspheres (Ni@PA6M) with Ni nanoparticles uniformly dispersed by the reaction induced phase separation (RIPS) method, then mixed with MWCNT and PS at high speed and formed by hot pressing. Under the opti-