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

1
Wigner Research Centre for Physics, Hungarian Academy of Sciences, Konkoly-Thege Miklós út 29-33, 1121 Budapest, Hungary
2
Hevesy György PhD School of Chemistry, Eötvös Loránd University, Pázmány Péter sétány 1/A, 1117 Budapest, Hungary
3
Department of Materials Physics, Eötvös Loránd University, Pázmány Péter sétány 1/A, 1117 Budapest, Hungary
*
Author to whom correspondence should be addressed.
Crystals 2019, 9(7), 334; https://doi.org/10.3390/cryst9070334
Received: 24 May 2019 / Revised: 26 June 2019 / Accepted: 26 June 2019 / Published: 28 June 2019
(This article belongs to the Special Issue Recent Progress in Lithium Niobate)
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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. View Full-Text
Keywords: lithium niobate; high-energy ball-milling; nanocrystals; mechanochemical reaction lithium niobate; high-energy ball-milling; nanocrystals; mechanochemical reaction
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Kocsor, L.; Péter, L.; Corradi, G.; Kis, Z.; Gubicza, J.; Kovács, L. Mechanochemical Reactions of Lithium Niobate Induced by High-Energy Ball-Milling. Crystals 2019, 9, 334.

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