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The influence of the fuel (glycine, urea, citric acid and sucrose) and calcination temperature used to obtain calcium aluminate in the mayenite phase assisted by solution combustion synthesis (SCS) is the central point of this work. Thermal gravimetric analysis helps to establish the calcination temperatures used (1100, 1200 and 1300 °C). Using the X-ray diffraction technique (XRD) and complementary analyses, such as Raman spectroscopy, the specific surface area and laser granulometry, it was possible to elucidate the behavior and relationship of the fuel and heat treatment on the phase formation, crystallite size and powder crystallinity. Glycine showed better performance than other fuels, with the lowest calcination temperature, obtaining pure mayenite with nanometric crystallite size in all calcination ranges. Thus, it was observed that the type of fuel has an influence on obtaining pure mayenite, as well as the calcination temperature, and glycine reveals the best performance. [ABSTRACT FROM AUTHOR]