Synthesis of Nanoscale CaO-Al2O3-SiO2-H2O and Na2O-Al2O3-SiO2-H2O Using the Hydrothermal Method and Their Characterization

C-A-S-H (CaO-Al₂O₃-SiO₂-H₂O) and N-A-S-H (Na₂O-Al₂O₃-SiO₂-H₂O) have a wide range of chemical compositions and structures and are difficult to separate from alkali-activated materials. Therefore, it is difficult to analyze their microscopic properties directly. This paper reports research on the synthesis of C-A-S-H and N-A-S-H particles with an average particle size smaller than 300 nm by applying the hydrothermal method. The composition and microstructure of the products with different CaO(Na₂O)/SiO₂ ratios and curing conditions were characterized using XRD, the RIR method, FTIR, SEM, TEM, and laser particle size analysis. The results showed that the C-A-S-H system products with a low CaO/SiO₂ ratio were mainly amorphous C-A-S-H gels. With an increase in the CaO/SiO₂ ratio, an excess of Ca(OH)₂ was observed at room temperature, while in a high-temperature reaction system, katoite, C₄AcH11, and other crystallized products were observed. The katoite content was related to the curing temperature and the content of Ca(OH)₂ and it tended to form at a high-temperature and high-calcium environment, and an increase in the temperature renders the C-A-S-H gels more compact. The main products of the N-A-S-H system at room temperature were amorphous N-A-S-H gels and a small amount of sodalite. An increase in the curing temperature promoted the formation of the crystalline products faujasite and zeolite-P. The crystallization products consisted of only zeolite-P in the high-temperature N-A-S-H system and its content were stable above 70%. An increase in the Na₂O/SiO₂ ratio resulted in more non-bridging oxygen and the TO₄ was more isolated in the N-A-S-H structure. The composition and microstructure of the C-A-S-H and N-A-S-H system products synthesized by the hydrothermal method were closely related to the ratio of the raw materials and the curing conditions. The results of this study increase our understanding of the hydration products of alkali-activated materials.