Three-dimensional microscopy can be used to reveal the shape, distribution, and connectivity of three-dimensional (3D) features that lie buried within an opaque material. This article discusses several experimental techniques that can be used to generate 3D images. These include serial sectioning, focused ion beam tomography, atom probe tomography, and X-ray microtomography. Nine case studies are presented that represent the work of the various research groups currently working on 3D microscopy using serial sectioning and illustrate the variants of the basic experimental techniques. The article also discusses the techniques for reconstruction and visualization of 3D microstructures with advanced computer software and hardware.

This article reviews the characterization methods for producing 3-D microstructural data sets. The methods include serial sectioning by mechanical material removal method and focused ion beam tomography method. The article describes how these data sets are used in realistic 3-D simulations of microstructural evolution during materials processing and materials response. It also explains how the 3-D experimental data are actually input and used in the simulations using phase-field modeling and finite-element modeling.

The quantitative characterization of fracture surface geometry, that is, quantitative fractography, can provide useful information regarding the microstructural features and failure mechanisms that govern material fracture. This article is devoted to the fractographic techniques that are based on fracture profilometry. This is followed by a section describing the methods based on scanning electron microscope fractography. The article also addresses procedures for three-dimensional fracture surface reconstruction. In each case, sufficient methodological details, governing equations, and practical examples are provided.

The objective of quantitative metallography/stereology is to describe the geometric characteristics of the features. This article discusses the geometric attributes of microstructural features that can be divided into: the numerical extents and the number density of microstructural features; derived microstructural properties; feature specific size, shape, and orientation distributions; and descriptors of microstructural spatial clustering and correlations. It emphasizes on the practical aspects of the measurement techniques and applications. The article also provides information on the quantitative metallographic methods for estimation of volume fraction, total surface area per unit volume, and total length of per unit volume.