Reaction products formed during alkaline activation, with 8M NaOH solutions, of fly ashes have been characterized with Si-29 and Al-27 magic-angle spinning nuclear magnetic resonance (MASNMR) spectroscopy. In particular, the influence of curing conditions (time and temperature of reaction) has been analyzed. NMR results show the formation of amorphous tecto-silicates in which the amount of aluminum decreases in the two consecutive formed phases. The Si/Al ratio of zeolite precursor obtained at 85 C changes from 0.95 to 1.86 when curing time is increased from 5 h to 1 week. The evolution of the mechanical properties of prepared cements has also been discussed in terms of the phases formed and texture and morphology of samples.