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

Laura Kocsor, L. Péter, G. Corradi, Zsolt Kis, J. Gubicza, L. Kovács

Research output: Article

Abstract

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
JournalCrystals
Volume9
Issue number7
DOIs
Publication statusPublished - júl. 1 2019

Fingerprint

Ball milling
lithium niobates
balls
Lithium
Heat treatment
grinding
Gene Conversion
Aluminum Oxide
Tungsten carbide
Stainless Steel
Crucibles
heat treatment
Dynamic light scattering
Crystallization
Titration
X ray powder diffraction
Nanocrystals
Raman spectroscopy
optical reflection
darkening

ASJC Scopus subject areas

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

Cite this

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title = "Mechanochemical Reactions of Lithium Niobate Induced by High-Energy Ball-Milling",
abstract = "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.",
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AU - Kocsor, Laura

AU - Péter, L.

AU - Corradi, G.

AU - Kis, Zsolt

AU - Gubicza, J.

AU - Kovács, L.

PY - 2019/7/1

Y1 - 2019/7/1

N2 - 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.

AB - 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.

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KW - Nanocrystals

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