The possibility of obtaining a homogeneous mixture or producing solid solutions and intermetallic compounds of Fe and Al nanoparticles have been investigated by applying the simultaneous pulsed wire evaporation (S-PWE) method. Fe and Al wires having 0.45-mm diameter and 35-mm length were co-fed continuously into the explosion chamber where they were exploded simultaneously. The phase composition, particle shape, and specific surface area (SSA) of the Fe-Al nano powders were affected by varying the explosion conditions, e. g., the wire distance, the input energy, and the atmospheric gas. The synthesized powders consist of not only pure metals of Al and α-Fe but also large amounts of high-temperature phases (γ-Fe, FeAl), and traces of other intermetallics. These results lead to the conclusion that a fraction of each phase can be controlled to create mixture of pure metals or solid solutions and intermetallic compounds.