Nanocrystalline MgAl2O4 spinel powder was synthesized using metal nitrates and a polymer matrix precursor composed of sucrose and polyvinyl alcohol (PVA). The precursor and the calcined powders were characterized by simultaneous thermal analysis (STA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to XRD results, the inceptive formation temperature of spinel via this technique was between 600 and 700 degrees C. The calcined powder at 800 degrees C for 2 h has faced shaped morphology and its crystallite size is in the range of 8-12 nm. Further studies also showed that the amount of polymeric matrix to metal ions has significant influence on the crystallite size of synthesized magnesium aluminate spinel powder. (C) 2007 Elsevier Ltd. All rights reserved.