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 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 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 describes testing and characterization methods of ceramics for chemical analysis, phase analysis, microstructural analysis, macroscopic property characterization, strength and proof testing, thermophysical property testing, and nondestructive evaluation techniques. Chemical analysis is carried out by X-ray fluorescence spectrometry, atomic absorption spectrophotometry, and plasma-emission spectrophotometry. Phase analysis is done by X-ray diffraction, spectroscopic methods, thermal analysis, and quantitative analysis. Techniques used for microstructural analysis include reflected light microscopy using polarized light, scanning electron microscopy, transmission electron microscopy, energy dispersive analysis of X-rays, and wavelength dispersive analysis of X-rays. Macroscopic property characterization involves measurement of porosity, density, and surface area. The article describes testing methods such as room and high-temperature strength test methods, proof testing, fracture toughness measurement, and hardness and wear testing. It also explains methods for determining thermal expansion, thermal conductivity, heat capacity, and emissivity of ceramics and glass and measurement of these properties as a function of temperature.

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.

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 provides a clear but nonexhaustive description of the general principle of atomic emission, with a particular focus on instrumentation, and summarizes the main characteristics of the inductively coupled plasma optical emission spectrometer technique. Basic atomic theory as well as the instrument characteristics and their influence on the instrument performances are presented. The advantages, drawbacks, and developments of this technique are discussed, and, finally, alternative techniques and examples of applications are provided.

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

Inductively coupled plasma atomic emission spectroscopy (ICP-AES) is an analytical technique for elemental determinations in the concentration range of major to trace based on the principles of atomic spectroscopy. This article provides a description of the basic atomic theory, and explains the analytical procedures and various interference effects of ICP, namely, spectral, vaporization-atomization, and ionization. It provides a detailed discussion on the principal components of an analytical ICP system, namely, the sample introduction system; ICP torch and argon gas supplies; radio-frequency generator and associated electronics; spectrometers, such as polychromators and monochromators; detection electronics and interface; and the system computer with appropriate hardware and software. The article also describes the uses of direct-current plasma, and provides examples of the applications of ICP-AES.

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

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.

Ultraviolet/visible (UV/VIS) absorption spectroscopy is a powerful yet cost-effective tool that is widely used to identify organic compounds and to measure the concentration of principal and trace constituents in liquid, gas, and solid test samples. This article emphasizes the quantitative analysis of elements in metals and metal-bearing ores. The instrumentation required for such applications consists of a light source, a filter or wavelength selector, and some type of visual or automated sensing mechanism. The article examines common sensing options and provides helpful information on how to set up and run a variety of UV/VIS absorption tests.

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.

This article focuses on the modes of operation, physical basis, sample requirements, properties characterized, advantages, and limitations of the characterization methods used to evaluate the physical morphology and chemical properties of component surfaces for medical devices. These methods include light microscopy, scanning electron microscopy, atomic force microscopy, energy-dispersive X-ray spectroscopy, Auger electron spectroscopy, secondary ion mass spectrometry, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy.

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 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.

This article describes the analytical methods for analyzing surfaces for corrosion and corrosion inhibition processes as well as failure analysis based on surface structure and chemical identity and composition. The principles and applications of the surface-structure analysis techniques, namely, optical microscopy, scanning electron microscopy, scanning tunneling microscopy, and atomic force microscopy, are reviewed. The article discusses the principles and applications of chemical identity and composition analysis techniques. These techniques include the energy dispersive X-ray spectroscopy, Auger electron spectroscopy, X-ray photoelectron spectroscopy, ion scattering spectroscopy, reflectance Fourier transform infrared absorption spectroscopy, Raman and surface enhanced Raman spectroscopy, and extended X-ray absorption fine structure analysis.