New synthesis process to prepare nano-particles of lithium niobate, sodium niobate and potassium niobate by thermal decomposition of the constituent double metal alkoxides was developed. Single crystals of such double-metal alkoxides as Na-Nb, Li-Nb and K-Nb ethoxides were newly synthesized from a mixed solution of the constituent metal ethoxides. The doublemetal alkoxides of the Li-Nb, Na-Nb and K-Nb systems decomposed at low temperatures below 673 K to form nano-particles of LiNbO3, NaNbO3 and LiNbO3. The lattice constants and crystallite size of the obtained LiNbO3, NaNbO3 and LiNbO3 particles were elucidated. It was shown that this new synthesis process was useful for preparation of niobate nano-particles at low temperatures.