This work presents a new synthesis of nano-sized lithium niobate particles by a low temperature three steps procedure. The complete protocol implies a LiH induced reduction of NbCl5 followed by in situ spontaneous oxidation into low valence niobium nano-oxides. These niobium oxides are exposed to air atmosphere leading to pure Nb2O5 formation. Finally, the stable Nb2O5 is converted into lithium niobate LiNbO3 nanoparticles during the controlled hydrolysis of the LiH excess. The nano-sized lithium niobate particles as well as their formation processes were characterized using X-ray photoelectron spectroscopy.
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