The synthesis of potassium hexafluoronickelate(Ⅳ) on the condition of high temperature and high pressure and its decomposition at high temperature have been studied. The result showed that fluorine gas can be quickly absorbed by a mixture of potassium fluoride and nickel fluoride at temperature above 225 ℃ and pressure of about 2 0 MPa. The FT IR spectra and Raman spectra verified the formation of potassium hexafluoronickelate(Ⅳ). When the temperature is raised to 250 ℃, potassium hexafluoronickelate(Ⅳ) will be decomposed to produce fluorine gas with a pressure reaching to 620 kPa at 350 ℃. The purity of fluorine is higher than 99%. It is suggested that potassium hexafluoronickelate(Ⅳ) can be used as a fluorine source.