Abstract: Single-phase nanocrystalline intermetallic compound AlNi particulate composite was synthesized by flow-levitation method. The morphology, granularity and phase structure of particles were investigated by TEM and XRD techniques. Results show that the grain size of the nanocrystalline intermetallic compound AlNi particulate is less than 40 nm. The data of chemistry elementary analysis indicate Al in nanoparti-culate up to 49%. Moreover, the formation mechanism of single-phase nanocrystalline intermetallic compound by flow-levitation method was also evaluated.