Al2O3 nanoparticles were prepared by polyethylene glycol octylphenyl ether(Triton X-100)/n-butyl alcohol/cyclohexane/ water W/O reverse microemulsion. The proper calcination temperature was determined at 1 150 ℃ by thermal analysis of the precursor products. The structures and morphologies of Al2O3 nanoparticles were characterized by X-ray diffraction, transmission electron microscopy and UV-Vis spectra. The influences of mole ratio of water to surfactant on the morphologies and the sizes of the Al2O3 nanoparticles were studied. With the increase of surfactant content, the particles size becomes larger. The agglomeration of nanoparticles was solved successfully. And the formation mechanisms of Al2O3 nanoparticles in the reverse microemulsion were also discussed.