Zircon whiskers were synthesized via non-hydrolytic sol-gel process combined with molten salt method by using anhydrous zirconium tetrachloride as zirconium source, TEOS as silicon source, anhydrous ethanol as solvent, and sodium molybdate as molten salt. The effects of heat treatment mode and cooling rate on the synthesis of zircon whiskers have been studied by means of XRD, FE-SEM, TG and TEM. The results indicate that well-developed whiskers can be prepared through heat treating the sample at 850°C for 3 h followed by a furnace cooling process. The zircon whiskers which were fabricated by this heat treatment mode grew along the [001] direction and showed diameter of 50~100 nm and aspect ratio of 20~30.