Encyclopedia of Glass Science, Technology, History, and Culture. Группа авторов
Thanks to P. Salmon for providing Figures 2a–c and constructive comments; D. Neuville for providing Figures 8 and 9; J.F. Stebbins, B.O. Mysen, L. Cormier, and G. Lelong for comments, suggestions, and keeping me on track with regard to the different techniques; and E.I. Kamitsos for providing me with a copy of his IR chapter prior to publication. Diffraction images provided courtesy of T. Höche of the Center for Applied Microstructure Diagnostics (CAM), Fraunhofer Institute for Mechanics of Materials IWM, Halle Germany.
References
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Note
1 Reviewers:B. Mysen, Geophysical Laboratory, Carnegie Institution of Washington, Washington, DC, USAJ. F. Stebbins, Geological and Environmental Sciences, Stanford University, Stanford, CA, USA
2.3 Microstructure Analysis of Glasses and Glass Ceramics
Christian Patzig and Thomas Höche
Fraunhofer Institute for Microstructure of Materials and Systems IMWS, Halle (Saale), Germany
1 Introduction
A homogeneous glass by definition lacks a microstructure at a scale larger than a few nanometers. As soon as actual inhomogeneities occur, in contrast, a detailed picture of their size, distribution, composition, and spatial arrangement becomes important to understand the properties of the material. In turn, the improved capabilities of microstructural studies in terms of spatial and elemental resolution are becoming increasingly important to optimize crystallization or phase separation and to achieve the desired microstructure and associated properties (Chapter 7.11). As a matter of fact, the beauty and challenge of glasses and glass ceramics is their diversity and complexity.
The purpose of this chapter thus is to review the main microstructural methods commonly used to study inhomogeneous glass‐based materials. In preamble, however, it is important to note that studying extremely small volumes in great detail can result in “knowing everything about nothing.” In other words, it is critically important to make sure that the information gathered locally is actually representative for larger volumes. To achieve this goal, highly resolved information must be combined with additional integral measurements to get a broad picture. In addition, artifacts introduced upon either preparation or investigation of the sample must be avoided. And one should also be extremely careful with in situ microstructural experiments where, because of dramatic differences in the surface‐to‐volume ratio, annealing can easily lead to results not observed in the bulk. For this reason, one is advised to freeze a microstructure evolution by stopping it at specific steps and to use multiple samples taken from different stages for gaining a “full‐picture” characterization.
When dealing with the early stages of crystallization or nanoscale phase separation, it is obvious that light microscopy is not an appropriate analysis technique because its optical resolution of a few 100 nm, which is limited by the wavelengths of visible light, is two