During the synthesis of geopolymer materials, all of the phenomena and reactions that occur should be included in the analysis of the synthesis. This work aims to study the role that siliceous species play in an activation solution in the presence of pure metakaolin. The formation of a gel phase during the synthesis of a K-geopolymer was shown. Different mixtures were analyzed by infrared spectroscopy. During material consolidation, there is always competition between the geopolymer network and the gel that is governed by a change in the siliceous species. The heat treatment of various gels and solids provided evidence of various networks in geopolymer materials. Finally, the change in the crystallinity of the silica in the activation solution led to a change in the kinetics of the polycondensation reactions, in agreement with previous work.