Multi-Spectroscopic Investigations for Comprehensive Structural Analysis of Aluminoborosilicate Glasses: I. Integrating Raman, XPS, XAS and NMR Techniques

Hanyu Hu; Sami Soudani; Jonathan Hamon; Nicolas Trcera; Michael Paris; Yann Morizet

doi:10.52825/glass-europe.v2i.1422

Authors

Hanyu Hu Institut des Matériaux Jean Rouxel https://orcid.org/0009-0001-4961-3954
Sami Soudani Institut des Matériaux Jean Rouxel https://orcid.org/0009-0001-9301-2566
Jonathan Hamon Institut des Matériaux Jean Rouxel
Nicolas Trcera Synchrotron soleil https://orcid.org/0000-0002-9364-1039
Michael Paris Institut des Matériaux Jean Rouxel https://orcid.org/0000-0002-8671-0630
Yann Morizet Institut des Matériaux Jean Rouxel https://orcid.org/0000-0001-9599-245X

DOI:

https://doi.org/10.52825/glass-europe.v2i.1422

Keywords:

Aluminoborosilicate Glasses, Raman Spectroscopy, XPS Spectroscopy, NMR Spectroscopy, XAS Spectroscopy

Abstract

For relatively simple glasses, such as binary or ternary glass systems, various characterization techniques have proven effective for determining network structures. However, structural analysis of multicomponent glass systems remains challenging due to complex network structures. In this study, we employed Raman, XPS, XAS, and NMR techniques to investigate the structure of soda lime aluminoborosilicate glasses. Our focus was on the polymerization degree of the silicate network (average Qⁿ value), the content of Non-Bridging Oxygen (NBO%), the connectivity between borate species (^[3]B-O-^[3]B% and ^[3]B-O-^[4]B%), and the chemical environment of Ca and Na cations. Raman spectral decomposition enabled the determination of the polymerization degree of the silicate network, which agreed well with the values calculated from ¹¹B and ²⁷Al NMR spectra for glasses without B-NBO species. XPS O1s spectra decomposition provided consistent NBO content values with those calculated from NMR results. The ¹¹B DQ-SQ NMR spectra can analyse the connectivity changes between borate species across different glass compositions. The ²³Na NMR spectra can provide a comprehensive view of the local environment of Na. The XAS spectra provided reliable insights into the local environment of Ca, detailing first shell configurations not easily obtained via NMR. We also presented an analysis scheme for ¹¹B NMR spectra to distinguish between ^[4]B(3Si,1B) and ^[4]B(4Si,0B) species. This study emphasizes the necessity of using a multi-spectroscopic approach to analyse the complex glass network structure.

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Multi-Spectroscopic Investigations for Comprehensive Structural Analysis of Aluminoborosilicate Glasses: I. Integrating Raman, XPS, XAS and NMR Techniques

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