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Abstract III–V semiconductor nanocrystals are an important class of optoelectronic materials. However, the gas‐phase synthesis of these materials, especially of the stibnides, has been left relatively unexplored. In this study, we demonstrate the synthesis of free‐standing GaSb nanocrystals for the first time, using a novel gas‐phase process. We show that when elemental aerosols are used as precursors for Ga and Sb, the elements mix at the nanometer length scale as the aerosols pass through a nonequilibrium plasma reactor. At sufficiently high plasma power, the mixing produces free‐standing GaSb nanocrystals, with a small amount of excess Ga segregated at the periphery of the particles. The reaction is initiated by vaporization of elemental aerosols in the plasma despite the low‐background temperature. Ion bombardment determines the extent of vaporization of Ga and Sb and thereby controls the ensemble stoichiometry and reaction rates.