A Comparative Overview of Glass-Ceramic Characterization by MAS-NMR and XRD

Abstract

Glass-ceramics are polycrystalline materials formed by controlled crystallization of parent glasses, which can be studied complementarily by XRD and NMR. XRD probes long-range order, while NMR is more element specific and probes the immediate environment around the atoms. These techniques allow considerable insights into the crystalline and amorphous constituents of glass-ceramics. In this article, we highlight some key issues in the characterization of glass-ceramics: phase identification and quantification, and structural characterization of the residual glass. The application of both NMR and XRD techniques are considered in these areas and their advantages and limitations discussed using our recent work and examples from the literature.

A method to quantify crystallinity in amorphous metal alloys: A differential scanning calorimetry study

“…Despite using a very slow scan rate in XRD, the patterns of amorphous SAM2×5 and SAM5% are very similar, thus it is impossible to quantify the crystallinity of SAM5% via XRD methods. This limitation is expected since the resolution of the XRD technique is about 5 wt.% for specimens without light-weight elements such as carbon and boron [72]. Lack of accuracy of XRD quantification becomes more significant for SAM2×5 materials, which have both boron and carbon at relatively high concentrations.…”

NMR Spectroscopy in Glass Science: A Review of the Elements

“…There continue to be a great number of significant and elaborate developments in the technique, including multi-nuclear correlations to expand the length-scale of structural understanding, the powerful combination of modeling and NMR experiments and other areas that lie outside the scope of this work. Past reviews on glass NMR have touched on many of these topics, including the comprehensive examination of NMR for different types of glasses by Eckert in 1992 [5], a recent summary of applications in glass-ceramic materials [6] and various specialized reviews on specific elements of interest or glass families [7,8,9]. …”

Structural mapping and tuning of mixed halide ions in amorphous sulfides for fast Li-ion conduction and high deformability

“…Amorphous matter, resembling a uid phase with an irregular and non-equilibrium arrangement of atoms from an atomistic viewpoint but having the physical form of a solid phase from a macroscopic viewpoint, is one of the most interesting material structures. [1][2][3][4][5][6][7][8] Through a combination of various glass formers and network modiers, this material offers the possibility of innite compositional diversity and property improvements without structural limitations. [1][2][3][4][5][6][7][8][9][10][11] Consequently, amorphous materials have been utilized in various industrial applications and are still being studied as promising next-generation materials.…”

“…[1][2][3][4][5][6][7][8] Through a combination of various glass formers and network modiers, this material offers the possibility of innite compositional diversity and property improvements without structural limitations. [1][2][3][4][5][6][7][8][9][10][11] Consequently, amorphous materials have been utilized in various industrial applications and are still being studied as promising next-generation materials. [9][10][11] In electrochemical phenomena and reactions involving mass transport, such as ions, this structure has various advantages due to its thermodynamically metastable phase.…”