Nanostructured materials have been largely studied in the last few years because they have a great potential to applications in different fields like physics, chemistry, biology, mechanic and medicine. Synthesis and characterization of nanostructured materials is a subject of great interest involving science, market, politicians, government and society. The nanostructured materials are in demand in biomedical area, mainly the bioceramics composed of calcium phosphates (Ca/P), which have an excellent biocompatibility and mineralogical characteristics similar to those of bones. The aim of this work was to optimize the method of powder synthesis of nanostructured calcium phosphate and of nanocomposites composed of calcium phosphate//SiO2n, containing 5, 10 and 15% (in volume) of nanometric silica (SiO2n). The results are expressed according to the method of synthesis, mineralogical and morphological characterization, and thermal behavior for the different compositions of the nanostructured powder synthesized.