Polymer-derived ceramics have drawn considerable attention for their flexibility to fabricate into diverse shapes such as fibers, ceramic foams or globes.Therefore, in this work, diverse Zr/Si/C polymer microspheres were prepared by polyzirconocenesilane, which were applied as the precursors to be sintered into Zr/Si/C ceramic microspheres.The pyrolytic process of polyzirconocenesilane and ceramization of polymer-derived Zr/Si/C ceramics were investigated by TGA, XRD, TG-FTIR, TG-GC-MS, SEM and EDS.Finally, the Zr/Si/C ceramic microspheres were successfully obtained after sintering at high temperature, mainly due to the high ceramic yield of preceramic polymer (66%-70%, at 800 ℃).Moreover, the morphology, microstructure and chemical composition of such polymer-derived Zr/Si/C ceramic microspheres were analysed by SEM and EDS.Such Zr/Si/C ceramic microspheres may perform attractive wave-absorbing properties and high gas sensitivity, which would be promising candidates for novel absorbents, special electronic devices, and gas sensors.