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.

Transmission electron microscopy (TEM) approach enables essentially simultaneous examination of microstructural features through imaging from lower magnifications to atomic resolution and the acquisition of chemical and crystallographic information from small regions of the thin specimen. This article discusses fundamentals of the technique, especially for solving materials problems. Background information is provided to help understand basic operations and principles, including instrumentation, the physics of signal generation and detection, image formation, electron diffraction, and spectrometry techniques with data analysis.

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 discusses the principles of physical metallurgy and metallography of depleted uranium. It describes the techniques involved in the preparation of thin foils for transmission electron microscopy and illustrates the resulting microstructure of uranium and uranium alloys, with the aid of black and white images. The article also provides information on the applications of etching and examination of uranium alloys, at both macro and micro scales, in characterizing the grain structures, segregation patterns, inclusions, and the metal flow geometries produced by solidification and mechanical working processes.

This article reviews the main theoretical and practical aspects of sequence normally followed in digital image-acquisition, processing, analysis, and output for material characterization. It discusses the main methods of digital imaging, image processing, and analysis, as applied to microscopy of materials. The article describes the basic concepts of sampling and resolution and quantization of light microscopy, scanning electron microscopy, and transmission electron microscopy. It discusses the acquisition of a digital image that accurately represents the sample under observation and output of the image to a printer. The methods used to enhance the digital image and to extract quantitative information are also described. Different types of image segmentation, namely, adaptive segmentation and contour-based segmentation, are reviewed. The article also presents case studies on the application of image processing and analysis to materials characterization.

This article discusses the specimen preparation of three types of cast and wrought heat-resistant alloys: iron-base, nickel-base, and cobalt-base. Specimen preparation involves sectioning, mounting, grinding, polishing, and etching. The article illustrates the microstructural constituents of cast and wrought heat-resistant alloys. It describes the identification of ferrite by magnetic etching. The transmission electron microscopy examination of the fine strengthening phases in wrought alloys and bulk extraction in heat-resistant alloys are included. The article also reviews the gamma prime phase, gamma double prime phase, eta phase, laves phase, sigma phase, mu phase, and chi phase in wrought heat-resistant alloys.

Anodizing is one of the most common surface treatments of aluminum and is performed for corrosion protection. This article describes the structure and growth characteristics of the types of anodic oxide films such as a barrier-type oxide film and a porous-type anodic oxide film. It discusses each step involved in the anodizing process of an aluminum or aluminum alloy specimen. The anodizing process includes pretreatments (degreasing, etching, and polishing), anodizing, coloring, and sealing. The article provides an observation of the morphology of the anodic oxide films by transmission electron microscopy and the scanning electron microscopy for testing properties of anodic oxide films.

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.

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.

The application of transmission electron microscope to the study of fracture surfaces and related phenomena has made it possible to obtain magnifications and depths of field much greater than those possible with light (optical) microscopes. This article reviews the methods for preparing single-stage, double-stage, and extraction replicas of fracture surfaces. It discusses the types of artifacts and their effects on these replicas, and provides information on shadowing of replicas. The article concludes with a comparison of the transmission electron and scanning electron fractographs with illustrations.

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.