Deuterated nitroguanidine （NQ-d₄） and deuterated 1，1-diamino-2，2-dinitroethylene （FOX-7-d₄） were synthesized via H/D exchange starting from nitroguanidine （NQ） and 1，1-diamino-2，2-dinitroethylene （FOX-7）. The target products were characterized by IR， NMR （¹H and ¹³C）， HPLC， TG-DTG， DSC and neutron diffraction. DSC/TG data show that the decomposition temperatures of NQ-d₄ and FOX-7-d₄ were 2.5 ℃ and 2.6 ℃ higher than those of NQ and FOX-7， respectively. The deuteration rates of NQ-d₄ and FOX-7-d₄ are respectively 95.27% and 98.87% as measured by neutron diffraction. The purities of NQ-d₄ and FOX-7-d₄ are respectively 99.51% and 99.28% obtained by HPLC via area normalization method.