Hierarchical structure porous MoS2/SiO2 microspheres were prepared by ultrasonic pyrolysis technique. The nanostructured MoS2/SiO2 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 MoS2/SiO2 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:SiO2 ratio on the hierarchical structure was also investigated. (c) 2011 Canadian Society for Chemical Engineering