MgAl 2 O 4 is the most important compound in the MgO–Al 2 O 3 system which can be produced through various methods. In the present work, synthesis and sintering behaviour of nano-sized spinel powder produced through mechano-chemical process were studied. For this purpose, MgCl 2 6H O, and NaOH reagents altogether with a small amount of water were mixed and subjected to high-energy ball milling for a short time (10 min). After confirming the occurrence of solid-phase displacement reactions by X-ray diffraction, the as-milled powders were washed, dried and then heated from 400 C to 1200 C for 2 h. The heated powders were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, simultaneous thermal analysis, BET and transmission electron microscopy techniques. It was found that pure nano-sized spinel phase, with 8–12 nm mean particle size and 76.9 m 2 /g specific surface area is obtainable through heating the precursor for 2 h at 800 C. The synthesized powders were sintered at 1500 C and obtained 93.8% of the theoretical density. 2 O, AlCl 3 6H 2