ZnO–Al 2O 3 mixed oxide nanoparticles were successfully produced from a solution containing Zn (acetate) and AlCl 3 by the solvothermal method. Calcination process of the ZnO–Al 2O 3 composite nanoparticles brought forth polycrystalline two-phase ZnO–Al 2O 3 nanoparticles of 30–50 nm in diameters. ZnO and Al 2O 3 were crystallized into würtzite and rock salt structures, respectively. Optical properties of ZnO–Al 2O 3 nanoparticles were determined with solid state UV and florescence (PL) spectroscopies. Structural properties of this sample were analyzed by XRD, SEM and Raman spectroscopy and then compared with bulk case of these samples.