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

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.