3,3′-Dicyano-4,4′-azofurazan (DCAF) was synthesized from 3-amino-4-aminoxim-idofurazan (AAOF) through two-step oxidization and the product was characterized by IR, NMR and elemental analysis. The crucial factors of KMnO₄ oxidization reaction were studied and the optimal reaction conditions were confirmed. The single crystal of DCAF was cultivated for the first time and tested by single-crystal X-ray diffraction. The crystal is triclinic, space group P-1 with crystal parameters a=1.8297(11) nm, b=0.588(3) nm, c=0.9069(5) nm, V=0.8853(9) nm^-3, Z=4, D_c=1.622 g·cm^-3, F (000)=432, μ (Mo Kα )=0.131 mm^-1, R₁=0.1039, wR =0.2420.