A high purity LiPF6 that has been widely used as lithium-ion secondary batteries electrolyte was prepared using acetonitrile as the medium. The target product was analyzed by FT-IR, TG-DTA and XRD, FT-IR. The results indicate the absorption brands of LiPF6 agreed reasonably with the theoretical predictions. TG-DTA showed that the decomposition of LiPF6 was in three steps in stead of one step.