Abstract: Cryolite-type fluoride K₃VF₆ was successfully synthesized under mild hydrothermal condition.The structure of the compound was determined by means of powder X-ray diffraction analysis.K₃VF₆ has a tetragonal cryolite-type structure with lattice parameter a=13.570 Å,b=13.570 Å,c=8.671 Å.The compound was further characterized by using scanning electron microscopy,thermogravimetric,differential thermal analysis.The variable temperature magnetic susceptibility of the compound was characterized and the result showed that the magnetic ordering was related to the crystallographic features and isolated magnetic unit with the temperature decreasing.