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Microstructure Evaluation and Impurities in La Containing Silicon Oxynitrides.
Abbas Saeed Hakeem1, Sharafat Ali2, Thomas Höche3,4
1Interdisciplinary Research Center for Hydrogen & Energy Storage (IRC-HES) Research Institute, King Fahd University of Petroleum & Minerals, Dhahran 31261, Saudi Arabia.
Nitrogen-rich La-Si-O-N glasses contain impurities like elemental silicon and metal silicides, causing opacity. These defects hinder commercialization, stemming from high-temperature reactions during glass synthesis.
Area of Science:
- Materials Science
- Glass Science
- Ceramics
Background:
- Oxynitride glasses remain largely uncommercialized due to inherent impurities.
- Nitrogen-rich lanthanum silicon oxynitride (La-Si-O-N) glasses present unique microstructural challenges.
Purpose of the Study:
- Investigate the microstructure and intrinsic defects in nitrogen-rich La-Si-O-N glasses.
- Identify the sources of opacity and impurities in these advanced glass materials.
Main Methods:
- Glass synthesis via high-temperature heating (1650-1800 °C) of La metal, Si3N4, and SiO2 in a nitrogen atmosphere.
- Microstructural and impurity analysis using optical microscopy, SEM, AFM, and TEM-EELS.
- Quantification of silicide particle content and characterization of elemental silicon formation.
Main Results:
- The synthesized La-Si-O-N glasses contained <2 vol.% spherical metal silicide particles (<1 µm).
- Opacity is attributed to elemental silicon from Si3N4/SiO2 decomposition above ~1600 °C and La-metal silicide intermetallics.
- No clear correlation found between silicide formation and glass composition or preparation temperature.
Conclusions:
- High-temperature reactions during synthesis lead to critical impurities (elemental Si, silicides) in La-Si-O-N glasses.
- These microstructural defects, particularly elemental silicon and silicides, are the primary cause of glass opacity.
- Addressing these impurity-related defects is crucial for the potential commercialization of oxynitride glasses.
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