This article is a detailed account of the principles of electron-excited X-ray microanalysis. It begins by discussing the physical basis of electron-excited X-ray microanalysis and the advantages and limitations of energy dispersive spectrometry (EDS) and wavelength dispersive spectrometry for electron probe microanalysis. Key concepts for performing qualitative analysis and quantitative analysis by electron-excited X-ray spectrometry are then presented. Several sources that lead to measurement uncertainties in the k-ratio/matrix corrections protocol are provided, along with the significance of the raw analytical total. Sections on accuracy of the standards-based k-ratio/matrix corrections protocol with EDS and processes of analysis when severe peak overlap occurs are also included. The article provides information on low-atomic-number elements, iterative qualitative-quantitative analysis for complex compositions, and significance of standardless analysis in the EDS software. It ends with a section on the processes involved in elemental mapping for major and minor constituents.

Electron probe microanalysis (EPMA) makes it possible to combine structural and compositional analysis in one operation. This article describes the basic concepts of microanalysis and the processing of EPMA that involves the measurement of the characteristic X-rays emitted from a microscopic part of a solid specimen bombarded by a beam of accelerated electrons. It provides information on the various aspects of energy-dispersive spectrometry (EDS) and wavelength-dispersive spectrometry (WDS), and elucidates the qualitative analysis of the major constituents of EDS and WDS. The article includes information on the analog and digital compositional mapping of elemental distribution, and describes the strengths and weaknesses of WDS and EDS spectrometers in X-ray mapping. It also outlines the application of EPMA for solving various problems in materials science.

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 briefly discusses popular techniques for metals characterization. It begins with a description of the most common techniques for determining chemical composition of metals, namely X-ray fluorescence, optical emission spectroscopy, inductively coupled plasma optical emission spectroscopy, high-temperature combustion, and inert gas fusion. This is followed by a section on techniques for determining the atomic structure of crystals, namely X-ray diffraction, neutron diffraction, and electron diffraction. Types of electron microscopies most commonly used for microstructural analysis of metals, such as scanning electron microscopy, electron probe microanalysis, and transmission electron microscopy, are then reviewed. The article contains tables listing analytical methods used for characterization of metals and alloys and surface analysis techniques. It ends by discussing the objective of metallography.

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.

This article focuses on the visual or macroscopic examination of damaged materials and interpretation of damage and fracture features. Analytical tools available for evaluations of corrosion and wear damage features include energy dispersive spectroscopy, electron probe microanalysis, Auger electron spectroscopy, secondary ion mass spectroscopy, and X-ray powder diffraction. The article discusses the analysis and interpretation of base material composition and microstructures. Preparation and examination of metallographic specimens in failure analysis are also discussed. The article concludes with a review of the evaluation of polymers and ceramic materials in failure analysis.

This article introduces various analytical techniques commonly used in the characterization of organic solids and liquids and discusses the challenges in performing the analysis, with examples. Some general advice in approaching a material analysis is also provided.

This article describes some of the common elemental composition analysis methods and explains the concept of referee and economy test methods in failure analysis. It discusses different types of microchemical analyses, including backscattered electron imaging, energy-dispersive spectrometry, and wavelength-dispersive spectrometry. The article concludes with information on specimen handling.

This article provides an overview of how this volume is organized and structured. It describes the methods for analyzing the materials in simplified terms and emphasizes the most common applications and limitations of each method.

The characterization, testing, and nondestructive evaluation of ceramics and glasses are vital to manufacturing control, property improvement, failure prevention, and quality assurance. This article provides a broad overview of characterization methods and their relationship to property control, both in the production and use of ceramics and glasses. Important aspects covered include the means for characterizing ceramics and glasses, the corresponding rationale behind them, and relationship of chemistry, phases, and microconstituents to engineering properties. The article also describes the effects that the structure of raw ceramic materials and green products and processing parameters have on the ultimate structure and properties of the processed piece. The effects that trace chemistry and processing parameters have on glass properties are discussed. The article describes mechanical tests and failure analysis techniques used for ceramics.

Scanning electron microscopy (SEM) has unique capabilities for analyzing fracture surfaces. This article discusses the basic principles and practice of SEM, with an emphasis on its applications in fractography. The topics include an introduction to SEM instrumentation, imaging and analytical capabilities, specimen preparation, and the interpretation of fracture features. SEM can be subdivided into four systems, namely, illuminating/imaging, information, display, and vacuum systems. The article also describes the major criteria and techniques of SEM specimen preparation, and the general features of ductile and brittle fracture modes.

This article provides an overview of how fractographs in this Atlas are organized and presented. It contains a table that lists the distribution content of illustrations for various materials discussed in the Atlas. The causes of fractures for various ferrous and nonferrous alloys and engineered materials are also illustrated.

X-ray spectroscopy is generally accepted as the most useful ancillary technique that can be added to any scanning electron microscope (SEM), even to the point of being considered a necessity by most operators. While “stand-alone” x-ray detection systems are used less frequently in failure analysis than the more exact instrumentation employed in SEMs, the technology is advancing and is worthy of note due to its capability for nondestructive analysis and application in the field. This article begins with information on the basis of the x-ray signal. This is followed by information on the operating principles and applications of detectors for x-ray spectroscopy, namely energy-dispersive spectrometers, wavelength-dispersive spectrometers, and handheld x-ray fluorescence systems. The processes involved in x-ray analysis in the SEM and handheld x-ray fluorescence analysis are then covered. The article ends with a discussion on the applications of x-ray spectroscopy in failure analysis.

Scanning electron microscopy (SEM) has shown various significant improvements since it first became available in 1965. These improvements include enhanced resolution, dependability, ease of operation, and reduction in size and cost. This article provides a detailed account of the instrumentation and principles of SEM, broadly explaining its capabilities in resolution and depth of field imaging. It describes three additional functions of SEM, including the use of channeling patterns to evaluate the crystallographic orientation of micron-sized regions; use of backscattered detectors to reveal grain boundaries on unetched samples and domain boundaries in ferromagnetic alloys; and the use of voltage contrast, electron beam-induced currents, and cathodoluminescence for the characterization and failure analysis of semiconductor devices. The article compares the features of SEM with that of scanning Auger microscopes, and lists the applications and limitations of SEM.

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.

This article uses metal and alloy powders as examples to briefly discuss how to perform the characterization of powders. It begins by reviewing some of the techniques involved in the sampling of powders to ensure accurate characterization. This is followed by a discussion on the important properties to characterize powders, namely the particle size, surface area, density, porosity, particle hardness, compressibility, green strength, and flowability. For characterization of powders, both individual particles and bulk powders are used to evaluate their physical and chemical properties. The article also discusses the important characteristics and compositions of powder as well as impurities that directly affect powder properties. It ends with a description of the ignition and dust-explosion characteristics of organic and metal powders.

This article provides detailed information on the instrumentation and principles of the scanning electron microscope (SEM). It begins with a description of the primary components of a conventional SEM instrument. This is followed by a discussion on the advantages and disadvantages of the SEM compared with other common microscopy and microanalysis techniques. The following sections cover the critical issues regarding sample preparation, the physical principles regarding electron beam-sample interaction, and the mechanisms for many types of image contrast. The article also presents the details of SEM-based techniques and specialized SEM instruments. It ends with example applications of various SEM modes.