Double-perovskite Sr2Fe1-xScxMoO6- (x = 0, 0.05, 0.1, 0.2, 0.3, 0.4) powders have been synthesized by sol-gel citrate method. Initial powders were calcined in different temperature and atmosphere (air, H2(4vol%)/Ar), then analyzed by using the methods of X-ray, scanning electron microscopy (SEM), as well as thermal analysis. It is found that the formation of perovskite structure is related to the content of Sc, pH value, calcination temperature and sintering atmosphere. Especially, a pure perovskite structure almost completely formed after three hours sintering in atmosphere of H2(4vol%)/Ar. Although the formation of perovskite structure also happened in the air atmosphere, at the same time the SrMoO4 structure formed undesirably as a result of oxidization of Mo.