Nanocrystalline microstructure is regarded as a strategic approach to overcome the brittleness of alumina ceramics, and the preparation of disperse equiaxed α‐Al2O3 nanoparticles is an essential step for the preparation of nanocrystalline alumina ceramics. In this work, disperse equiaxed α‐Al2O3 nanoparticles were prepared using α‐Fe2O3 as seed and isolation phase. At first, the composite of α‐Al2O3 nanoparticles embedded in α‐Fe2O3 matrix was obtained by calcining the precursor powder containing γ‐AlOOH and Fe(OH)3 (Fe3+/Al3+ mole ratio of 5) at 770°C for 2 h. Then disperse equiaxed α‐Al2O3 nanoparticles with a mean size of 12 nm and a size distribution from 2 to 40 nm without vermicular microstructure were obtained by removal of α‐Fe2O3 and other impurities in the composite through acid corrosion.