The Electron-Optical Investigation of Clays
Clay minerals occur most frequently in a state too finely divided for satisfactory observation with the best optical microscopes, or for study with single-crystal X-ray techniques. The higher resolution made possible by electron-optical instruments can therefore be put to good use in the investigation of the morphologies and crystal structures of clays. It is the intention of this monograph to summarize achievements to date, to indicate problems that have perhaps not received the attention they deserve, and, as a result, to suggest lines of investigation that might prove fruitful. The first two chapters explain in some detail the various types of electron-optical equipment that are currently available, the methods of operating them to the best advantage, and interpretation of the results. The techniques for preparation of specimens are reviewed in the third chapter, with emphasis on those most suitable for clay minerals. With the exception of the last chapter, on practical applications of electron-optical methods, each subsequent chapter deals with studies on a particular class of clay minerals. Some chapters include detailed descriptions of specimen preparation or other techniques that have been developed by the authors to resolve specific problems peculiar to the minerals dealt with in those chapters. Electron microscopy and other electron-optical techniques have been used, alone or in conjunction with other methods, to investigate problems that have proved otherwise insoluble. Nevertheless, these techniques have their limitations, which must always be borne in mind, as results can occasionally be misleading. It therefore seems appropriate, at this stage, to review the methods of specimen preparation and examination, and to attempt to assess their value for investigation of clays.
Resolution and contrast in an electron microscope image are dependent in part upon several factors in the selection or preparation of the specimen over which the electron microscopist has some control. For example, there are various ways of observing the specimen: as a dispersed powder; as a thin section; and indirectly by the use of surface replicas. One cannot expect the same limits of resolution for each of these methods, and even within each method the resolving power and contrast vary with specimen thickness, film thickness, stability of the specimen, and stability of the supporting film or replica. In order to establish some basis for selecting one method over the other, a brief discussion of some of the problems peculiar to the preparation techniques used in electron microscopy will be given. The techniques described are intended only as a guide. The individual must decide what method is best for his particular specimen and may often have to modify existing methods.
Because of the need to evacuate the lens column and specimen chamber to pressures in the range of 10-4 mm Hg, the specimen must be in a dry state. In this connection it must be noted that even the presence of thin films of organic materials oflow volatility can have a harmful effect by contributing to the formation of a carbonaceous film at the surface of the specimen due to breakdown of the structure in the electron beam; such films can seriously reduce contrast in the image and impair resolution.