The geopolymerization process of metakaolinite activated by alkali and alkali silicate solutions was revealed. The effects of alkali concentration, modulus of alkali silicate solution and reaction temperature on geopolymerization were Studied systematically by isothermal calorimetry, as well as X-ray diffraction and Al-27/Si-29 MAS NMR. Results show that the geopolymerization process of metakaolinite under alkali activation condition can he reasonably supposed into three stages: (I) destruction, (II) polymerization and (III) stabilization. The rate of geopolymerization in KOH solution is higher than in NaOH solution and reaches the maximum in 15 mol/L KOH solution during stage II. The extent of geopolymerization increases with increasing of alkali content regardless of the existence of silicate anions in activator. (C) 2009 Elsevier B.V. All rights reserved.