Structural Unit Determination in Silica Nanoparticles Using Infrared Micro-Reflectance Spectroscopy

Appl Spectrosc. 2024 Feb;78(2):209-216. doi: 10.1177/00037028231218289. Epub 2023 Dec 21.

Abstract

A method based on infrared (IR) micro-reflectance measurements for the structural characterization of glassy nanomaterials is presented. Near-specular reflectance spectra of pressed pellets can be analyzed using a model relating the structure of silicate glasses to their dielectric response and an effective medium approximation to account for the effect of porosity. The integrated intensities of phenomenological bands attributed to Q2, Q3, and Q4 structural units allow quantifying their relative populations. These values are in good agreement with those obtained with magic-angle spinning nuclear magnetic resonance, which serves as validation of the method and proves the feasibility of extracting quantitative information about glass structure from IR micro-reflectance experiments.

Keywords: Infrared spectroscopy; effective medium theories; glass structure; infrared microscopy; sol-gel silica.