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La2Mo2O9 nanocrystallites were synthesized successfully using Sol-gel process with (NH4)6Mo7O24·4H2O,La(NO3)3·6H2O,citric acid and PEG400 as original materials.The result shows that spherical well-crystallized La2Mo2O9 nanoparticles were formed at 500℃ with sizes of ca.80 and 20nm,which indicates the secondary nucleation exists in the reaction process.The synthesized La2Mo2O9 nanocrystallites were characterized by XRD,TEM,IR and UV-Vis spectrum,respectively.