Mixed amorphous and crystalline MgAl2O4 nanopowders with visible light-induced photocatalytic activity were prepared via a simple solution combustion method using glycine and urea as fuel mixtures. The obtained samples were characterized by X-ray diffraction, field emission scanning electron microscopy, energy-dispersive X-ray, transmission electron microscopy, Brunauer-Emmett-Teller (BET) surface area, thermogravimetry. X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and UV-Vis diffuse reflection spectrum. The results showed that the combustion was almost complete, the crystallinity and crystallite size of MgAl2O4 increased with the increase of fuels, and there was N atoms doped in the catalysts. The MgAl2O4 containing amorphism had photo-absorption ability in visible light region. The photocatalytic results for degradation of methylene blue (MB) indicated that the combustion-synthesized samples had photocatalytic activity, whereas the annealed well crystalline MgAl2O4 nanopowders had none. The MgAl2O4 sample containing about 45.6% crystalline and 55.4% amorphous materials showed the highest photocatalytic activity, with a 99.5% MB removal in 100 min under visible light irradiation. The fluorescence spectra verified that the greater the formation rate of center dot OH radicals, the higher the photocatalytic activity achieved. (C) 2011 Elsevier B.V. All rights reserved.