Abstract

The crystallization of glass microspheres in the Y2O3–Al2O3-system produced from precursor powders of four different nominal compositions via flame synthesis is analyzed in detail by electron microscopy with a focus on electron backscatter diffraction (EBSD). Growth models are formulated for individual microspheres crystallized during flame synthesis as well as after an additional heat treatment step. 16 different types of crystallized bodies are cataloged for future reference. They are presented without regard for their relative occurrence; some are extremely rare but illustrate the possibilities of flame synthesis in the analyzed system. All three phases in the binary Y2O3–Al2O3-phase diagram (Y3Al5O12, YAlO3 and Y4Al2O9) and α-alumina are located by EBSD. Energy dispersive X-ray spectrometry results obtained from these microspheres show that their chemical composition can deviate from the nominal composition of the precursor powder. The multitude of differing microsphere types showing polygon and dendritic crystal growth as well as phase separation indicate that flame synthesis can lead to a wide variety of parameters during microsphere production, e.g. via irregular flight paths through the flame, contaminants or irregular cooling rates.

Highlights

  • The crystallization of glass microspheres in the ­Y2O3–Al2O3-system produced from precursor powders of four different nominal compositions via flame synthesis is analyzed in detail by electron microscopy with a focus on electron backscatter diffraction (EBSD)

  • Various microstructures in cross sections of microspheres have been presented using ­SEM18–21, they have never been analyzed in detail using EBSD which was only recently applied to a microsphere containing YAG​21

  • The results presented above show that the melt forming this sphere crystallized at a very high temperature while cooling from the outside, which is in agreement with the lack of any heat treatment after production

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Summary

Introduction

The crystallization of glass microspheres in the ­Y2O3–Al2O3-system produced from precursor powders of four different nominal compositions via flame synthesis is analyzed in detail by electron microscopy with a focus on electron backscatter diffraction (EBSD). While YAG has been crystallized from multiple glasses, their crystallization e.g. in glasses containing S­ iO2 often does not lead to the sole formation of YAG7​–9 or shows a low nucleation ­rate[10]. Both effects are problematic with respect to the transparency of the resulting materials. Powders of various nominal compositions in the Y­ 2O3–Al2O3-system have been prepared using a combination of the Pechini m­ ethod[26] and flame synthesis to enhance the chemical h­ omogeneity[18,19,20,21]

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