A method for the simple and efficient microwave radiation-assisted hydrothermal synthesis of Fe-2(MoO4)(3) has been developed. Several factors such as pH, addition rate, molybdenum precursor, type of solvent and various other microwave synthesis parameters are studied. The catalysts were characterized using X-ray diffraction, scanning electron microscopy, Mossbauer spectroscopy and specific surface area measurements. The results show that different morphologies can be obtained, depending on the conditions under which the iron molybdate is prepared. Nevertheless, in all cases the solid particles appear to be covered by an amorphous oxide layer, which is less rich in iron than in the case of a crystallized oxide layer. The presence of this amorphous layer was revealed on all facets of the molybdate, with approximately the same composition and thickness. In an effort to evaluate the relationship between the morphology of iron molybdate particles and their catalytic properties, several samples exhibiting different morphology were tested for the oxidation of propene to acrolein. These samples were tested for the oxidation of propene to acrolein. The catalysts with platelets morphology and exhibiting larger surface of (100) planes appeared more active. This was attributed to a faster re-oxidation due to the preferential diffusion of oxygen anions in the bulk structure channels perpendicular to these planes.