In this article, we review focused ion beam serial sectioning microscopy paired with analytical techniques, such as electron backscatter diffraction or x-ray energy-dispersive spectrometry, to study materials chemistry and structure in three dimensions. These three-dimensional microanalytical approaches have been greatly extended due to advances in software for both microscope control and data interpretation. Samples imaged with these techniques reveal structural features of materials that can be quantitatively characterized with rich chemical and crystallographic detail. We review these technological advances and the application areas that are benefitting. We also consider the challenges that remain for data collection, data processing, and visualization, which collectively limit the scale of these investigations. Further, we discuss recent innovations in quantitative analyses and numerical modeling that are being applied to microstructures illuminated by these techniques.

In situ observation is of great value in the study of radiation damage utilizing electron or ion irradiation. We summarize the facilities and give examples of work found around the world. In situ observations of irradiation behavior have fallen into two broad classes. One class consists of long-term irradiation, with observations of microstructural evolution as a function of the radiation dose in which the advantage of in situ observation has been the maintenance of specimen position, orientation, and temperature. A second class has involved the recording of individual damage events in situations in which subsequent evolution would render the correct interpretation of ex situ observations impossible. In this review, examples of the first class of observation include ion-beam amorphization, damage accumulation, plastic flow, implant precipitation, precipitate evolution under irradiation, and damage recovery by thermal annealing. Examples of the second class of observation include single isolated ion impacts that produce defects in the form of dislocation loops, amorphous zones, or surface craters, and single ion impact-sputtering events. Experiments in both classes of observations attempt to reveal the kinetics underlying damage production, accumulation, and evolution.

The focused ion beam (FIB) tool has been successfully used as both a stand alone analytical instrument and a means to prepare specimens for subsequent analysis by SEM, TEM, SIMS, XPS, and AUGER. In this work, special emphasis is given to TEM specimen preparation by the FIB lift-out technique. The fundamental ion/solid interactions that govern the FIB milling process are examined and discussed with respect to the preparation of electron transparent membranes. TRIM, a Monte Carlo simulation code, is used to physically model variables that influence FIB sputtering behavior. The results of such computer generated models are compared with empirical observations in a number of materials processed with an FEI 611 FIB workstation. The roles of incident ion attack angle, beam current, trench geometry, raster pattern, and target-material-dependent removal rates are considered. These interrelationships are used to explain observed phenomena and predict expected milling behaviors, thus increasing the potential for the FIB to be used more efficiently with reproducible results.