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.

The development of quantitative fractography (QF) parameters basically requires topological data of a fracture surface that can be derived from the stereological analysis of multiple projected scanning electron microscope (SEM) images; the profilometry-based techniques that measure the fracture surface profile along x-y sections of a fracture surface from metallographic sections or nondestructive techniques; and the three-dimensional reconstruction of the fracture surface topology using imaging methods such as stereo SEM imaging and confocal scanning laser microscopy. These three general methods of assessing fracture surface topology are reviewed in this article.

Field ion microscopy (FIM) can be used to study the three-dimensional structure of materials, such as metals and semiconductors, because successive atom layers can be ionized and removed from the surface by field evaporation. The ions removed from the surface by field evaporation can be analyzed chemically by coupling to the microscope a time-of-flight mass spectrometer of single-particle sensitivity, known as the atom probe (AP). This article describes the principles, sample preparation, and quantitative analysis of FIM. It also provides information on the principles, instrument design and operation, mass spectra and their interpretation, and applications of AP microanalysis.

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.

This article provides information on the general structural features and origins of metals. The characteristic structural features of single-phase metals and alloys, such as grain structure and substructure, are discussed. The article also describes the major types of multiphase structures and macrostructure of metals and alloys.

Metal transparency and interaction with X-rays have been recognized as obvious candidate principles from which methods for in situ monitoring of solidification processes could be developed. This article describes the use of X-ray imaging-based techniques to investigate interface morphology evolution, solute transport, and various process phenomena at spatiotemporal resolutions. It discusses the three viable imaging techniques made available by synchrotron radiation for the real-time investigation of solidification microstructures in alloys. These include two-dimensional X-ray topography, two-dimensional X-ray radiography, and ultra-fast three-dimensional X-ray tomography.

This article is an overview of the division Surface Analysis of this volume. The division covers various developed surface-analysis techniques, such as scanning probe and atomic force microscopy. The division focuses on the analysis of surface layers that are less than 100 nm. A quick reference summary of surface-analysis methods is presented in this article.

This article describes the determination of wear loss by measuring either mass change or dimensional change of lubricants and materials. It discusses the principles, advantages and disadvantages of mass loss measures and dimensional measures of wear. The article details wear measurement at the nanoscale, such as atomic force microscopy (AFM) measurement and scanning electron microscopy measurement. It reviews the techniques of wear measurement at the atomic level, namely, transmission electron microscopy (TEM) measurement and AFM combined with TEM measurement.

This article focuses on laboratory atomic force microscopes (AFMs) used in ambient air and liquid environments. It begins with a discussion on the origin of AFM and development trends occurring in AFM. This is followed by a section on the general principles of AFM and a comprehensive list of AFM scanning modes. There is a brief description of how each mode works and what types of applications can be made with each mode. Some of the processes involved in preparation of samples (bulk materials and those placed on a substrate) scanned in an AFM are then presented. The article provides information on the factors applicable to the accuracy and precision of AFM measurements. It ends by discussing the applications for AFMs in the fields of science, technology, and engineering.

This article demonstrates the depth and breadth of commercial and third-party software packages available to simulate metals processes. It provides a representation of the spectrum of applications from simulation of atomic-level effects to manufacturing optimization. The article tabulates the software name, function or process applications, vendor or developer, and website information.

Microstructure and crystallographic texture are the key material features used in the continuous endeavor to relate the processing of a metal with its final properties. This article emphasizes several aspects of deformation microstructures, namely, microstructural evolution, dislocation boundaries, and macroscopic properties. It discusses three different microstructural types: cell blocks, TL blocks, and equiaxed subgrains. The article also emphasizes the behavior of metals and single-phase alloys processed under plastic deformation (dislocation slip) conditions. It provides information on the microstructural parameters, measurement techniques, and microstructural relationships, which assist in predicting the mechanical properties and recrystallization behavior of materials. The article concludes with an analysis of the general relationship between the microstructural parameters and properties.

As additive manufacturing (AM) gains maturity as a manufacturing technique for production in many industrial sectors, inspection as a tool for quality control gains importance. This article is focused on the field of dimensional metrology, which is typically concerned with the verification of size, location, form, and surface topography of geometric features. This is split into two categories: geometric (size, location, form) and surface measurement (topography). The article also focuses on applicable inspection technologies, and it discusses the context within digital thread manufacturing. A case study on the Digital Inspection Requirements Enhancing Coverage and Traceability (DIRECT) is also presented.

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.

This article outlines the beam/sample interactions and the basic instrumental design of a scanning electron microscopy (SEM), which include the electron gun, probeforming column (consisting of magnetic electron lenses, apertures, and scanning coils), electron detectors, and vacuum system. It discusses the contrasts mechanisms used for imaging and analyzing materials in the SEM. These include the topographic contrast, compositional contrast, and electron channeling pattern and orientation contrast. Special instrumentation and accessory equipment used at elevated pressures and during the X-ray microanalysis are reviewed. The article also provides information on the sample preparation procedure and the materials applications of the SEM.