The synthesis of ceramic materials from polymeric precursors has been the subject of numerous studies due to lower energy cost compared to conventional processing. The study aims to research and develop synthesis of calcium aluminate powders via the polymeric precursor method, in order to obtain the pure phase of hepta-aluminate dodecálcio (C12A7) with mayenita mineral name, since it has applications like: special cements and components for high temperature fuel cells. A study of the evolution of crystalline phases by X-ray diffraction was performed, the vibrational modes of atomic location in crystalline phases were studied by micro-Raman spectroscopy was also performed and images from scanning electron microscopy. From the characterizations carried out on the material can be seen that the sintering temperature of 1200°C was obtained pure phase, so the choice of synthesis shown to be effective due to the complexity of obtaining this phase pure.