This article is intended to provide the reader with a good understanding of the underlying science, technology, and the most common applications of focused ion beam (FIB) instruments. It begins with a survey of the various types of FIB instruments and their configurations, discusses the essential components, and explains their function only to the extent that it helps the operator obtain the desired results. An explanation of how the components of ion optical column shape and steer the ion beam to the desired target locations is then provided. The article also reviews the many diverse accessories and options that enable the instrument to realize its full potential across all of the varied applications. This is followed by a detailed analysis of the physical processes associated with the ion beam interacting with the sample. Finally, a complete survey of the most prominent FIB applications is presented.

The introduction of focused ion beam (FIB) microscopy in the 1990s added the capability of studying fracture surfaces in the third dimension and making site-specific and stress-free transmission electron microscope (TEM) specimens in situ. This article reviews the methods for preparing replicas and the site-specific FIB thin-foil preparation technique. It provides an overview of FIB-TEM specimen preparation.

This article discusses the capabilities and limitations of various material characterization methods that assist in the selection of a proper analytical tool for analyzing particulate materials. Commonly used methods are microanalysis, surface analysis, and bulk analysis. The techniques used for performing microanalysis include scanning electron microscopy and electron probe X-ray microanalysis. The article describes surface analysis techniques, including Auger electron spectroscopy, X-ray photoelectron spectroscopy, and ion-scattering spectroscopy. Bulk analysis techniques, such as X-ray powder diffraction, inductively coupled plasma atomic emission spectroscopy, atomic absorption spectroscopy, and atomic fluorescence spectrometry, are also discussed.

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 describes the operation and capabilities of surface analysis methods of metals, including scanning electron microscopy, electron probe microanalysis, transmission electron microscopy, secondary ion mass spectroscopy, and X-ray photoelectron spectroscopy. It provides information on the capabilities, typical uses, spatial resolution, elemental analysis detection threshold and precision, limitations, sample requirements, and operating principles of the scanning auger microprobe.

This article is a compilation of terms and definitions related to materials characterization.

Microstructural analysis is the combined characterization of the morphology, elemental composition, and crystallography of microstructural features through the use of a microscope. This article reviews three types of the most commonly used electron microscopies in metallurgical studies, namely scanning electron microscopy, electron probe microanalysis, and transmission electron microscopy. It briefly describes the operating principles, instrumentation which includes energy dispersive X-ray detectors, spatial resolution, typical use of the techniques, elemental analysis detection threshold and precision, limitations, sample requirements, and the capabilities of related techniques.

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.

Spark source mass spectrometry (SSMS) is an analytical technique used for determining the concentration of elements in a wide range of solid samples, including metals, semiconductors, ceramics, geological and biological materials, and air and water pollution samples. This article discusses the basic principles of spark source technique; SSMS instrumentation such as ion source, electric sector, and magnetic sector; sample preparation; and test procedures of SSMS. Some of the related techniques to SSMS are laser ionization mass spectrometry and laser-induced resonance ionization mass spectrometry. The ions produced in SSMS are detected by either the photometric method or electrical detection method and quantitatively measured by techniques such as internal standardization techniques, isotope dilution, multi element isotope dilution, and dry spike isotope dilution. The detected spark source spectrum contains all the elemental data of the tested sample. Finally, the article exemplifies the applications of SSMS.

This article presents a basic overview of technology-driven advances in the imaging of primarily metallic fracture surfaces. It describes various types of microscopes, including scanning electron, dual-beam, ion source, and transmission electron microscopes, and their capabilities. It also covers other useful hardware, such as computer-aided tomography (CAT) and micro-computer-aided tomography (micro-CAT) instruments. The article introduces some of the fracture image postprocessing methods and software, including image registration or alignment, focus stacking, Z-stacking, focal plane merging, and image stitching.

Surface modification is the alteration of the surface composition or structure using energy or particle beams. This article discusses two different surface modification methods. The first, ion implantation, is the introduction of ionized species into the substrate using kilovolt to megavolt ion accelerating potentials. The second method, laser processing, is high-power laser melting with or without mixing of materials precoated on the substrate, followed by rapid melt quenching. The article also describes the advantages and disadvantages of the surface modification approach to promote corrosion resistance.

This article discusses the operating principles, advantages, and limitations of scanning electron microscopy, atomic force microscopy, x-ray photoelectron spectroscopy, and secondary ion mass spectroscopy that are used to analyze the surface chemistry of plastics.

This article focuses on a variety of laser beam machining (LBM) operations of aluminum and its alloys, namely, laser cutting, laser drilling, laser milling, laser turning, laser grooving, laser scribing, laser marking, and laser micromachining. It presents different approaches for carrying out machining operations, laser processing parameters, efficiency and accuracy of the process, and the effect of laser processing parameters on the quality of the machined surface. The article provides an overview of the various conventional (chip forming) and nonconventional machining techniques employed for aluminum-based materials. A comparison of the various aspects of LBM with other non-conventional techniques is also presented. The article also describes the features of LBM techniques employed for aluminum and its alloys for different types of machining.

Analytical transmission electron microscopy (ATEM) is unique among materials characterization techniques as it enables essentially the simultaneous examination of microstructural features through high-resolution imaging and the acquisition of chemical and crystallographic information from small regions of the specimen. This article illustrates the effectiveness of the technique in solving materials problems. The first section of the article provides information on analytical electron microscope (AEM) and its basic operational characteristics as well as on electron optics, electron beam/specimen interactions and the generation of a signal, signal detectors, electron diffraction, imaging, x-ray microanalysis, electron energy loss spectroscopy, and sample preparation. The second section consists of 12 examples, each illustrating a specific type of materials problem that can be solved, at least in part, with AEM.