Institute of Metals Division - The Observation of Dislocations and Other Imperfections by X-Ray Extinction Contrast

ABOUT twenty-seven years ago W. bergl discovered that interesting detail could be seen in an X-ray diffraction spot made with a rock-salt crystal if the recording photographic film were held very close to the reflecting crystal. He also showed that much of this detail could be explained in terms of the deformation structure of the specimen. In the same year, 1931, Fox and parr2 reported that X-ray reflections from a quartz crystal were much more intense while the crystal was undergoing piezoelectric oscillation than when it was at rest. This observation was soon confirmed (and explained in terms of X-ray extinction) by Barrett3 in the United States and by Nishikawa et a1.,4 in Japan. During the next few years Barrett refined Berg's method for making X-ray diffraction micrographs and applied it to the study of metallic crystals. He reported this work in the 1945 annual lecture of the AIME.5 Since 1945 relatively little use has been made of the Berg-Barrett (B-B) method for making diffraction micrographs, though considerable interest in investigating subcrystal structures by other methods has developed. Some of these methods depend upon evaporation6 or chemical etching7 and, therefore, suffer from the occasional intrusion of subtle artifacts such as those recently reported by Hooker for leada and Welsh for aluminum.9 Other methods require the introduction of foreign elements which "decorate" the substructure in some way, thereby rendering it detectable by direct" or indirect1'. visual examination. Still others depend upon complex and often highly questionable analyses of X-ray diffraction line profiles. There have also been a number of related X-ray techniques, such as the Lambot,12 Schulz13 and Merlini and Guinier,14 which have proved to be quite useful for specific applications. Some of these methods give a picture of the substructure which is more or less directly related to the shape and the topography of the specimen. The Berg-Barrett method carries this desirable feature to the limit. Closely related to the B-B method are three photographic X-ray techniques recently described by Lang.15 These methods give beautiful pictures of the internal structure of crystals but are limited by the facts that the required apparatus is rather complex, exposure times are long, and the specimen crystals must be thin. An experimental appraisal which I have recently made of the original B-B method has shown that this simple technique is not only inexpensive and convenient, but can give more information than was apparently realized by its inventors. For example, first-order subgrains in iron-silicon crystals were clearly delineated and their relative orientation subject to description. Also defect structures could be seen within the subgrains and in some materials slip bands could be clearly seen with respect to the topography of the rest of the specimen. This much had already been described by Barrett. However, in the present study it was found that the actual sites of individual dislocations which emerge upon the crystal surface could be located. Furthermore, by a simple procedure, the direction (but not sign) of the dislocation Burgers' vector could be defined as well.