3, 3′-Bis(tetrazol-5-yl)-4, 4′-azofurazan(DTZAF) was synthesized from 3-amino-4-(tetrazol-5-yl)furazan, and its four energetic salts were then synthesized via metathesis reaction with total yield of 73.0%, 70.3%, 75.0%, 76.3%. Theri structures were characterized by IR, ¹³C NMR, ¹H NMR, MS and elemental analysis. Their thermal decomposition products were studied by TG-DSC-IR-MS. The thermal prpperties of DTZAF and its energetic salts were studied by differential scanning calorimetry(DSC) and thermogravimetry(TG). Results show that DTZAF and its energetic salts have good thermal stability before 200 ℃.