The key intermediate diazidoglyoxime(DAG) of synthesizing 5, 5′-bistetrazole -1, 1-diolate dihydrate(BTO) was synthesized by "one pot" method using glyoxime as starting materials. The potassium salts of 5, 5′-bistetrazole -1, 1′-diolate(PBTOX) was synthesized by metathesis reaction. Its structure was characterized by IR and elemental analysis. DTA-TG technique was used to study the thermal decomposition of PBTOX. The surface morphology and mechanical properties of PBTOX crystal were tested by atomic force microscopy(AFM) and Lorentzian contact resonance(LCR) imaging technique. The sensitivity tests were performed. Results show that the crystal structure of PBTOX is layered one. Its decomposition peak temperature at a heating rate of 5 ℃·min^-1 is 383 ℃. Its explosion percentage is 0% for impact sensitivity and friction sensitivity.