Energetic crystals with nanoparticle inclusions were preparated and characterized, focusing on the nanosized iron(III) oxide-ammonium perchlorate system, generated using an ethyl acetate/acetone antisolvent:solvent system. It is shown that capture is dependent on antisolvent-to-solvent ratio; increased quantities of antisolvent lead to faster nucleation rates, smaller crystals, and improved capture. Additionally, the crystal habit formation is modified by the addition of nanoparticles, resulting in highly uniform rod-like crystal structures. Results with nanoaluminum-ammonium perchlorate and nanoaluminum-cyclotrimethylenetrinitramine (RDX) systems have shown similar capture behavior.