1,1-Diamino-2,2-dinitroethylene (C2H4N4O4, FOX-7) quasi-three-dimensional (3D) grids, a promising high-energy-density material with superior sensitivity properties, were synthesized by a spray freeze-drying technique. The FOX-7 3D grids were constructed from one-dimensional nanostructures. The sizes and structures of the FOX-7 3D grids strongly depend on the concentration of the aqueous solution of FOX-7. A possible formation mechanism of this structure was proposed in detail. Thermal analysis reveals that decrease in average particle sizes of FOX-7 grids results in a lower decomposition temperature and a much higher decomposition rate, which is in agreement with those reported about inorganic nanomaterials. (C) 2010 Elsevier B.V. All rights reserved.