Particle-induced x-ray emission (PIXE) is one of several quantitative analyses based on characteristic x-rays. This article provides a detailed account on the principles of PIXE, discussing the data-reduction codes used to identify, integrate, and reduce x-ray peaks into elemental concentrations. It provides information on the calibration of PIXE analysis, which is mostly performed using gravimetric standards to avoid serious absorption, refluorescence, or ion energy change corrections. A comparative study on PIXE and x-ray fluorescence is also included. Finally, the article discusses the applications of PIXE in three areas, namely, atmospheric physics and chemistry, external proton milliprobes and historical analysis, and PIXE microprobes.

This article provides a detailed account of particle-induced x-ray emission (PIXE), covering the basic principles of PIXE analysis and calibration and quality-assurance protocols employed. A comparative study on PIXE and x-ray fluorescence is then presented. The article also discusses the applications of PIXE in atmospheric physics and chemistry, external proton milliprobes and historical analysis, and PIXE microprobes.

The raw materials used in thermal spray processes are a critical parameter in the finished coating because the variations in their size, morphology, chemistry, and phase composition can significantly impact coating properties. Therefore, it is important to test and characterize the raw materials. This article discusses various characterization methods for powders. Topics discussed include: methods for determining particle size and/or size distribution; powder and coating stoichiometry; particle chemistry; and phase analysis by x-ray diffraction. This article discusses the characterization of thermal spray powders which involves the determination of particle size and/or size distribution and phase analysis by x-ray diffraction. It provides information on preferential volatilization and rapid solidification that influence compositional differences. Wet chemical methods, spectographic analysis, and atomic absorption spectrometry are also discussed.

This article provides an introduction to x-ray spectrometry, and discusses the role of electromagnetic radiation, x-ray emission, and x-ray absorption. It focuses on the instrumentation of wavelength-dispersive x-ray spectrometers, and energy dispersive x-ray spectrometers (EDS) that comprise x-ray tubes, the analyzing system, and detectors. The fundamentals of EDS operation are described. The article also provides useful information on preparation of various samples, explaining the qualitative and quantitative analyses of EDS. It reviews the applications of the x-ray spectrometry.

This article provides a detailed account of X-ray spectroscopy used for elemental identification and determination. It begins with an overview of the operating principles of X-ray fluorescence (XRF) spectrometer, as well as a comparison of the operating principles of wavelength-dispersive spectrometer (WDS) and energy-dispersive spectrometer (EDS). This is followed by a discussion on the mechanism and effects of X-ray radiation, X-ray emission, and X-ray absorption. The article then discusses components used, operation, and applications of WDS and EDS. Some of the factors and processes involved in sample preparation for XRF analysis are also included. The article further provides information on the practical procedure for and the applications of WDS and EDS qualitative and quantitative analyses.

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 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.

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.

The scanning electron microscopy (SEM) is one of the most versatile instruments for investigating the microstructure of metallic materials. This article highlights the development of SEM technology and describes the operation of basic systems in an SEM, including the electron optical column, signal detection and display equipment, and vacuum system. It discusses the preparation of samples for observation using an SEM and describes the application of SEM in fractography. If the surface remains unaffected and undamaged by events subsequent to the actual failure, it is often a simple matter to determine the failure mode by the use of an SEM. In cases where the surface is altered after the initial failure, the case may not be so straightforward. The article presents typical examples that illustrate these points. Image dependence on the microscope type and operating parameters is also discussed.

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.

This article provides a detailed account of the concepts and applications of neutron activation analysis (NAA), covering the basic principles and neutron reactions of NAA as well as calibration methods used for NAA. The discussion also covers the factors pertinent to analytical sensitivity achievable with NAA, common neutron sources, sample-handling technique, and automated systems of NAA. The categories of NAA covered are instrumental neutron activation analysis, epithermal neutron activation analysis, radiochemical neutron activation analysis, 14 MeV fast neutron activation analysis, delayed neutron activation analysis, and prompt gamma activation analysis.

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 describes the test techniques that are available for monitoring crack initiation and crack growth and for obtaining information on fatigue damage in test specimens. These techniques include optical methods, the compliance method, electric potential measurement, and gel electrode imaging methods. The article discusses the magnetic techniques that are primarily used as inspection techniques for detecting fatigue cracks in structural components. It details the principles and operation procedures of the liquid penetrant methods, positron annihilation techniques, acoustic emission techniques, ultrasonic methods, eddy current techniques, infrared techniques, exoelectron methods, and gamma radiography. The article explains the microscopy methods used to determine fatigue crack initiation and propagation. These include electron microscopy, scanning tunneling microscopy, atomic force microscopy, and scanning acoustic microscopy. The article also reviews the X-ray diffraction technique used for determining the compositional changes, strain changes, and residual stress evaluation during the fatigue process.

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.

This article describes the structure of coatings produced by plasma spraying, vapor deposition, and electrodeposition processes. The main techniques used for microstructure assessment are introduced. The relationship between the microstructure and property is also discussed. The experimental techniques for microstructural characterization include metallographic technique, X-ray diffraction, electron, microscopies, and porosimetry.

This article describes the applications, methods, and limitations of five principal nondestructive test methods, namely, penetrant testing, magnetic-particle testing, eddy current testing, radiographic testing, and ultrasonic testing. The article also provides guidance for the method selection for respective applications.

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.