Using dichloroglyoxime as raw material, dihydroxylammonium 5, 5′-bistetrazole-1, 1′-diolate (HATO) was synthesized via substitution, cyclization and metathesis reaction with a total yield of 81.7%. Wet diazidoglyoxime was experimentally found to increase the operational safety, and dilithium 5, 5′-bistetrazole-1, 1′-diolate with high solubility in water was employed to increase the yield of metathesis reaction. Further more, the properties of HATO such as thermal stability, mechanical sensitivity, morphology, size and particle distribution were investigated. It was found that the values of exothermic peak, standard volume of gas evolved, explosion probability of impact sensitivity, 50% drop height of impact sensitivity, explosion probability of friction sensitivity, and mean volume diameter are 249.14 ℃ (10 ℃·min^-1), 0.3 mL·g^-1(100 ℃/48 h), 16% (10 kg drop hammer, 25 cm drop height), 100 cm (5 kg drop hammer), 24% (3.92 MPa, 90 °), 334 μm.