Nanometric magnetic systems, such as ferrites, metallic oxides, and core@shell structures, represent a group of promising materials due to their extensive technological potential and the possibility of advancing our understanding of fundamental physics at the nanoscale. With this in mind, we synthesized core@shell nanoparticles CoFe2O4@NiO using an adapted coprecipitation method and systematically investigated the structural, morphological, and magnetic properties of this nanostructured system. We reported the achievement of core@shell nanostructures with pure phases through structural and morphological characterization. Through comprehensive experimental magnetic analysis, we evaluated the magnetic response of the precursor phases and the core@shell nanostructure. We identified the “wasp waist” behavior and the “exchange bias” effect, indicating exchange coupling between the phases at the interface. Ultimately, our findings allow us to consider the procedures employed, including adapted coprecipitation and calcination processes, as a viable route for producing high-quality core@shell nanostructures.