Synthesis and Characterization of 12CaO·7Al2O3 Slags: The Effects of Impurities and Atmospheres on the Phase Relations
Fabian Imanasa Azof, Kai Tang, Jinglin You, Jafar Safarian
Abstract
Abstract Synthesis of crystalline slags of 12CaO·7Al 2 O 3 phase from the corresponding melt compositions in different atmospheric conditions and different purities is investigated. Observations using a thermogravimetry coupled with differential thermal analysis showed that the dehydration of a zeolitic 12CaO·7Al 2 O 3 phase occur at 770 °C to 1390 °C before it congruently melts at 1450 °C. The X-ray diffraction pattern of the slag showed that a single 12CaO·7Al 2 O 3 phase is produced from a mixture, which has small SiO 2 impurity with a 49:51 mass ratio of CaO to Al 2 O 3 . A scanning electron microscope and electron probe micro-analyzer showed that a minor Ca-Al-Si-O-containing phase is in equilibrium with a grain-less 12CaO·7Al 2 O 3 phase. Moreover, 12CaO·7Al 2 O 3 is unstable at room temperature when the high-purity molten slag is solidified under oxidizing conditions contained in an alumina crucible. On the other hand, a high-temperature in-situ Raman spectroscopy of a slag that was made of a higher purity CaO-Al 2 O 3 mixture showed that 5CaO·3Al 2 O 3 phase is an unstable/intermediate phase in the the CaO-Al 2 O 3 system, which is decomposed to 12CaO·7Al 2 O 3 above 1100 °C upon heating in oxidizing conditions. It was found that 5CaO·3Al 2 O 3 is present at room temperature when the 12CaO·7Al 2 O 3 dissociates to a mixture of 5CaO·3Al 2 O 3 , 3CaO·Al 2 O 3 , and CaO·Al 2 O 3 phases during the cooling of the slag at 1180 °C ± 20 °C in reducing atmosphere. It is proposed that low concentrations of Si stabilize 12CaO·7Al 2 O 3 (mayenite), in which Si is a solid solution in its lattice, which is named Si-mayenite. Regarding the calculated CaO-Al 2 O 3 -SiO 2 diagram in this study, this phase may contain a maximum of 4.7 wt pct SiO 2 , which depends on the total SiO 2 in the system and the Ca/Al ratio.