The influence of doping on the structural and morphological properties of the phosphor system, obtained ultrasonically via Spray Pyrolysis from common gadolinium and europium nitrate solutions, was studied. The particle morphology, crystalline and chemical structure were studied by XRD, SEM and EDS. TEM was applied in order to identify the structure and growth of "primary nanoparticles" and determine the presence of domains locally affected by "Moires Frames" and "Crystallite Size". The SADP allows determining the presence of a polycrystalline material with two phases in the "as-prepared" samples, and only an Ia3 phase along the thermal treatment.