Preparation of a high purity powder is one of the most important steps in making transparent MgAl2O4 ceramic. Additionally, the particles require to have nanoscale scale, uniform particle size and least agglomeration, which make the diffusion enhanced at grain boundary during sintering process, promote densification to achieve full dense bulk material. In the present work, solution combustion synthesis was carried out to prepare MgAl2O4 nanopowder from magnesium nitrate hydrate (Mg(NO3)2.6H2O) and aluminum nitrate hydrate (Al(NO3)3.9H2O) as oxidizers and urea CH4N2O as fuel. The obtained powders present agglomerates of nanoscale particles.The average particle size of the obtained powder was about 20 nm. Investigation of the influence of the milling processing on the deagglomeration efficiency and the properties of the sintered sample showed that increasing milling time and ball-to-weight ratio led to reduce aggglomerate size and fraction, consequently, enhanced significantly shrinkage value, relative density and compressive strength of the sintered MgAl2O4. The relative density and the compressive strength achieved highest values of 98% and 155 MPa, respectively, regarding to the powder with milling condition of 48h milling time and 30/1 ball-to-powder ratio.