Ion exchange of glass has been utilized to give various functionalities to the melt-quenched glass, where the size effects between the exchanged ions often play important roles like chemical strengthening of glass. However, the smallest monovalent cations of H⁺ and D⁺ have not been well investigated as a counter cation of the ion-exchange pair. They are bare of the electron shell (empty 1s orbital) and would show different interaction phenomena with anions like oxygens in the glass network from alkali ions. In this study, the ion-exchange treatments of H⁺ or D⁺ with the smallest alkali ion of Li⁺ were conducted on lithium aluminosilicate glasses. Dipping and field-assisted methods were used as the ion-exchange technique. Non-bridging oxygen-free (NBO-free) glasses of Li₂O-Al₂O₃-SiO₂ system were prepared using melt-quenching method. The platelet glass samples were subjected to the ion exchange at 290-300 ^oC using conc-H₂SO₄ or D₂SO₄ as the sources of H⁺ or D⁺, respectively. Dipping and field-assisted methods gave the different ion-exchange ratios, and the latter enabled the fully ion exchange of glass samples with H⁺ or D⁺ without crack. The fully ion-exchanged samples showed low thermal expansivity below 400 ^oC and shrinkage at higher temperature due to the release of water from the glass network. The structural analysis using Infrared and Raman spectroscopies and nuclear magnetic resonance (NMR) spectroscopy were carried out on the samples. Some of the incorporated H or D were found to form H₂O or D₂O molecules in the glasses accompanying with the structural evolutions; the rearrangement of the network of TO₄ tetrahedra and the increase of the oxygen coordination number of Al³⁺ ions. In the presentation, the analysis results of ¹H/²⁹Si and ¹H/²⁷Al CP-MAS-NMR results and the measured properties of the ion-exchanged glass samples are shown to consider the ion-exchange phenomena in glass.

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