Abstract:A technique of environment scanning electron microscope(ESEM) was used to in situ quantitatively observe and record the hydration process of K-PSDS geopolymer matrix under RH 80%. The ESEM micrographs and corresponding EDXA show that metakaolinite grains pile up loosely at 10 min after mixing, which lead to many large voids. As hydration proceeds, a lot of gel is seen and is gradually precipitated on these grain surfaces. At late stage, these grains are packed by thick gel layers, and voids are fully filled. In situ studies on K-PSDS matrix by EDXA display that the values of n(K_2O)/n(Al_2O_3) and n(SiO_2)/n(Al_2O_3) are continuously reduced with the development of hydration, the values of n(K_2O)/n(Al_2O_3) and n(SiO_2)/n(Al_2O_3) of hydration products at 9 h after mixing are 1.28 and 6.54 respectively, which are near to the theoretical values (1.0, 6.0). In addition, well-developed crystals are not found at any ages, while sponge-like gel is always been observed.