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.
Highlights
Lithium niobate (LN, LiNbO3 ) crystals have countless non-linear optical and acoustic applications due to their versatile optical and ferroelectric properties
All of them have a broad distribution in the range of a few hundred nanometers while the smallest particle diameter can be achieved by the ball-milling in stainless steel vial
Nano-LN was prepared by ball-milling using a Spex 8000 Mixer Mill with different milling parameters
Summary
Lithium niobate (LN, LiNbO3 ) crystals have countless non-linear optical and acoustic applications due to their versatile optical and ferroelectric properties. In recent decades nanocrystalline materials have attracted considerable interest as their properties greatly differ from their coarse-grained counterparts. Nonlinear optical nanocrystals may have many applications such as building blocks of coherent subwavelength light sources [2,3,4,5,6] and nonresonant markers in second harmonic generation microscopy [4,7,8]. Rare-earth-doped LN nanocrystals could play an important role in coherent quantum optical experiments, e.g., as single photon sources, providing sharply defined wavelengths [9,10]. Many wet chemical synthesis methods are known for the preparation of nanocrystalline materials
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