文摘
Room temperature and high temperature x-ray powder diffraction and differential thermal analysis/thermo-gravimetric analysis (DTA/TGA) have been used to characterize the phase evolution of bulk mayenite (Ca12Al14O33) prepared using the citrate sol-gel method. These studies have shown that single phase mayenite forms at 900 掳C in air after approximately three hours. High temperature x-ray powder diffraction data show that when firing in air at temperatures 600 掳C and below only amorphous content is observed; above 600 掳C CaCO3 is the first phase to crystallize. For samples quenched at 800 掳C and evaluated using room temperature x-ray powder diffraction mayenite, CaAl2O4, and CaCO3 were present. High temperature x-ray diffraction data collected while firing in 4% H2/96% N2 reveals that CaCO3 does not form and Ca12Al14O33 starts to form around 850 掳C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method support the complete decomposition of metastable phases and the formation of mayenite at 900 掳C, although the phase evolution is different depending on the environment.