
High purity tetrafluorohydrazine is synthesized by reacting NF.sub.3 with silicon at an elevated temperature. The reaction occurs only periodically and at a low concentration of NF.sub.3. Immediate cooling of the reaction material produces tetrafluorohydrazine and SiF.sub.4. Alkaline hydrolysis removes substantially all impurities. Tetrafluorohydrazine is further recovered by cryogenic trapping from the remaining impurities.











