Effects of quartz particle size and water-to-solid ratio on hydrothermal synthesis of tobermorite studied by in-situ time-resolved X-ray diffraction

Hydrothermal synthesis process of tobermorite (5CaO·6SiO2·5H2O) has been investigated by in-situ X-ray diffraction using high-energy X-rays from a synchrotron radiation source in combination with a purpose-build autoclave cell. Dissolution rates of quartz were largely affected by its particle size distribution in the starting mixtures. However, the composition (Ca/Si) of non-crystalline C–S–H at the start of tobermorite formation was identical regardless of the quartz dissolution rate. An effect of water-to-solid ratio (w/s) was investigated for samples using fine particle quartz. Tobermorite did not occur with w/s of 1.7 but occurred with w/s higher than 3.0. Surprisingly, however, the dissolution curves of quartz were nearly identical for all samples with w/s from 1.7 to 9, indicating that the dissolution rate is predominated by surface area. Possible reaction mechanism for tobermorite formation will be discussed in terms of Ca and/or silicate ion concentration in the liquid phase and distribution of Ca/Si in non-crystalline C–S–H.

Graphical abstractTime-resolved XRD data set was obtained at up to 190 °C under a saturated steam pressure. Tobermorite (5CaO·6SiO2·5H2O) formation reaction was investigated in detail for several different starting materials.Figure optionsDownload full-size imageDownload as PowerPoint slideHighlights► Hydrothermal formation of tobermorite was monitored by in-situ XRD. ► Ca/Si of C–S–H at the start time of tobermorite formation was determined. ► The Ca/Si value was identical regardless of the quartz particle size in the starting mixture.