Potassium titanoniobate (KTiNbO 5 ) polycrystalline powders were synthesized by the sol–gel method and a novel preparation route which was described as a combination technique of the sol–gel process and solvothermal treatment. The synthesis processes, the structure and morphology characterizations for the as-prepared KTiNbO 5 particles were investigated by using thermal analysis, X-ray powder diffraction, electron microscopy and other techniques. The KTiNbO 5 particles synthesized in this work showed various morphologies depending on the different reaction processes. The KTiNbO 5 compound obtained through 2-propanol solvothermal treatment exhibited unique particle morphology characteristic of sphere shape with the average size of 300 nm in diameter. In addition, the result that the formation of the spherical particle shape occurred during the solvothermal process was demonstrated.