We describe a new laboratory‐scale aerosol process for making submicrometer AIN powder by reaction of gas phase Al(C2H5)3and NH3. The process can produce spherical, near‐stoichiometric AIN powder with mean particle diameter ranging from 0.07 to 0.20 μm and polydispersity index between 0.2 and 0.5. The inlet TEA concentration is found to have the greatest effect on particle size, with the furnace temperature and carrier gas flow rate having lesser influence. Our results appear to favor a LaMer‐type mechanism (particle nucleation, followed by condensation growth) over fusion‐coalescence to explain particl