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Nanocrystallization in Oxyfluoride Glasses Controlled by Amorphous Phase Separation.

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  • 1Otto-Schott-Institut für Materialforschung, Jena University , Fraunhoferstraβe 6, 07743 Jena, Germany.

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|August 28, 2015
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Summary

Researchers created transparent glass-ceramics with ZnF2, K2SiF6, and KZnF3 nanocrystals. The study reveals that controlling initial liquid-liquid phase separation in oxyfluoride glasses allows tuning the size and crystal phase of the resulting nanocrystals.

Keywords:
K2SiF6KZnF3Nanocrystallizationglass-ceramicoxyfluoride glassphase separation

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Area of Science:

  • Materials Science
  • Glass Science
  • Nanotechnology

Background:

  • Transparent glass-ceramics offer unique optical and mechanical properties.
  • Controlling nanocrystal formation within glass matrices is crucial for tailoring material characteristics.
  • Oxyfluoride glasses provide a versatile base for incorporating various functional nanocrystals.

Purpose of the Study:

  • To synthesize transparent bulk glass-ceramics containing specific fluoride nanocrystals (ZnF2, K2SiF6, KZnF3).
  • To investigate the influence of glass composition on crystallization behavior and microstructure.
  • To establish a correlation between initial phase separation and the final nanocrystal properties.

Main Methods:

  • Synthesis of xKF-xZnF2-(100 - 2x)SiO2 oxyfluoride glasses.
  • Heat treatment for controlled nucleation and crystal growth.
  • Replica transmission electron microscopy (TEM) for microstructure analysis.
  • Differential thermal analysis (DTA) to study thermal properties like glass transition temperature.

Main Results:

  • Successfully obtained transparent glass-ceramics with ZnF2, K2SiF6, and KZnF3 nanocrystals.
  • Crystallization behavior was found to be highly sensitive to glass composition (x = 20 to 22.5 mol %).
  • Liquid/liquid phase separation was observed, leading to distinct droplet and interpenetrating microstructures.
  • Fluoride depletion in the residual glass during crystallization was noted, potentially affecting viscosity.

Conclusions:

  • Initial liquid-liquid phase separation in multicomponent oxyfluoride glasses is a key factor in controlling nanocrystal formation.
  • The size and crystal phase of precipitated crystallites can be precisely tuned by manipulating the initial phase separation.
  • This work presents a novel method for fabricating tailored transparent glass-ceramics with embedded nanocrystals.