A new method for the synthesis of disodium dimolybdate (Na2Mo2O7) in the process of ultrasonic spray pyrolysis using acidified aqueous solutions of thermodynamically stable molybdenum (VI) oxide clusters as a precursor is described. Na2Mo2O7 particles were collected in alcohols (ethanol, 2-propanol, isobutyl alcohol), and ultracentrifugation was used to isolate solid material from solution. Scanning electron microscopy revealed the formation of uniform spherical Na2Mo2O7 particles with an average diameter of about 0.25 mu m. The X-ray diffraction analysis undoubtedly confirmed the formation of orthorhombic Na2Mo2O7 for samples synthesized at a temperature as low as 300 degrees C.