Mechanochemical Reactions of Lithium Niobate Induced by High-Energy Ball-Milling

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Lithium niobate (LiNbO3, LN) nanocrystals were prepared by ball-milling of the crucible residue of a Czochralski grown congruent single crystal, using a Spex 8000 Mixer Mill with different types of vials (stainless steel, alumina, tungsten carbide) and various milling parameters. Dynamic light scattering and powder X-ray diffraction were used to determine the achieved particle and grain sizes, respectively. Possible contamination from the vials was checked by energy-dispersive X-ray spectroscopy measurements. Milling resulted in sample darkening due to mechanochemical reduction of Nb (V) via polaron and bipolaron formation, oxygen release and Li2O segregation, while subsequent oxidizing heat-treatments recovered the white color with the evaporation of Li2O and crystallization of a LiNb3O8 phase instead. The phase transformations occurring during both the grinding and the post-grinding heat treatments were studied by Raman spectroscopy, X-ray diffraction and optical reflection measurement, while the Li2O content of the as-ground samples was quantitatively measured by coulometric titration.

Original languageEnglish
Article number334
Issue number7
Publication statusPublished - Jul 2019



  • High-energy ball-milling
  • Lithium niobate
  • Mechanochemical reaction
  • Nanocrystals

ASJC Scopus subject areas

  • Chemical Engineering(all)
  • Materials Science(all)
  • Condensed Matter Physics
  • Inorganic Chemistry

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