The nanocrystalline sodium niobate(NaNbO 3 ) and sodium tantalite(NaTaO 3 ) powders with perovskite structure were synthesized by the solvthermal method with glycol as solvent. These powders were characterized by powder X-ray diffraction(XRD), Raman spectroscopy, Scanning electron microscopy (SEM) and transmission electron microscopy(TEM). Rietveld refinement of X-ray diffraction data and Raman spectroscopy confirm that the nanoparticles of NaNbO 3 and NaTaO 3 have orthorhombically distrorted structures with Pmc2 1 and Pbnm space groups, respectively.The SEM photograph shows that NaNbO 3 and NaTaO 3 powder are cubic morphology. The TEM and the SAED pattern confirmed that the nanoscale NaTaO 3 is single-crystal structure. In addition, the influence of the concentration on the NaTaO 3 powder characteristics was also detailed investigated.