Fe 3 O 4 /CNTs nanocomposites, which were prepared by polyol-medium in situ high-temperature decomposition of Fe(acac) 3 using PVP as stabilizing agent and modified with SDS, were further decorated with high-quality ZnS nanocrystal via a wet technique in glycol solution. The obtained ZnS/Fe 3 O 4 /CNTs nanohybrids were characterized by XRD, FT-IR, Raman microscope, TEM, EDS, XPS, VSM and fluorophotometers. Results indicated that magnetic Fe 3 O 4 nanoparticles and fluorescent ZnS nanocrystal were uniformly dispersed on the surface of CNTs layer-by-layer with PVP and SDS as stabilizing agent and ion-capture agent, respectively. The novel multi-functional nanohybrids exhibit super-paramagnetic properties with a saturation magnetization about 6•795 emu g −1 at room temperature and show a strong emission band at 367 nm with a broad shoulder around 342-483 nm due to the interactions and/or background emissions of Fe 3 O 4 and CNTs. The superparamagnetic and fluorescent properties of obtained products are promising for potential applications in magnetically guided and fluorescence tracing drug delivery systems.