Nanocrystalline MgAl2O4 spinel powder was synthesized by the urea-formaldehyde (UF) polymer gel combustion route. A transparent gel formed from magnesium nitrate, aluminium nitrate and UF after drying underwet self-sustained combustion when initiated with a burning splinter. The combustion product on calcinations at 850 degrees C formed MgAl2O4 spinel. Calcination of the combustion product resulted in particle coarsening. The powder obtained by planetary ball milling of the spinel had a median particle size of 1.58 mu m. The spinel particles are agglomerates of nanocrystallites of size in the range 10-30 nm. The compacts prepared by uni-axial pressing of the spinel powder sintered to >99% TD at 1600 degrees C. (C) 2008 Elsevier Ltd. All rights reserved.