Hierarchical structure porous MoS 2 /SiO 2 microspheres were prepared by ultrasonic pyrolysis technique. The nanostructured MoS 2 /SiO 2 materials were characterised by scanning electron micrograph (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), high-resolution transmission electron microscope (HRTEM), as well as nitrogen isotherm. The MoS 2 /SiO 2 microspheres, synthesised using polystyrene latex spheres as a template, showed two pore sizes: 5.8 and 68 nm. The micro-, meso-and macropore volume was also calculated. Effect of PSL:SiO 2 ratio on the hierarchical structure was also investigated.