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 endeavors to familiarize the reader with a selection of different ionization designs and instrument components to provide knowledge for sorting the various analytical strategies in the field of solid analysis by mass spectrometry (MS). It begins with a description of the general principles of MS. This is followed by sections providing a basic understanding of instrumentation and discussing the operating requirements as well as practical considerations related to solid sample analysis by MS. Instrumentation discussed include the triple quadrupole mass spectrometer and the time-of-flight mass spectrometer. Inductively coupled plasma and thermal ionization MS provide atomic information, and direct analysis in real-time and matrix-assisted laser-desorption ionization MS are used to analyze molecular compositions. The article describes various factors pertinent to ionization methods, namely glow discharge mass spectrometry and secondary ion mass spectrometry. It concludes with a section on various examples of applications and interpretation of MS for various materials.

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.

Homogenization, in a broad sense, refers to the processes designed to achieve uniform distribution of solutes or phases in a given matrix. This article addresses the root cause for inhomogeneities in cast components. It is nearly a standard industrial practice to homogenize alloys before thermomechanical processing. The article lists the objectives of homogenization and benefits of homogenization treatments. The benefits include increased resistance to pitting corrosion, increased resistance to stress-corrosion cracking, improved ductility, and uniform precipitate distribution during subsequent aging. The article provides a schematic illustration of an energy-dispersive X-ray spectroscope (EDS) scattered data of solute distributions across a dendrite due to microsegregation of chromium and molybdenum. It concludes with information on the computational modeling for simulation of microsegregation of chromium and molybdenum.

Leak testing is used to determine the rate at which a liquid or gas penetrates from inside a component or assembly to the outside, or vice versa. This article discusses the type of leaks, namely real leaks, and virtual leaks. It describes the leak testing of fluid systems at pressure through acoustic method and bubble testing. The article gives a short note on types of leak detectors, sulfur hexafluoride detectors and mass-spectrometer. It tabulates the pressure and vacuum system leak-testing methods and discusses the application of gas detectors in leak testing.

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.

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.

Gas chromatography/mass spectrometry (GC/MS) is useful in analyzing mixtures of organic compounds. This article commences with a description of the principles of mass spectrometry and gas chromatography. It provides information on the procedures of mass spectrum interpretation, and describes the experimental procedure of and sample preparation for GC/MS. The article also discusses complementary techniques, such as high-performance liquid chromatography/mass spectrometry and mass spectrometry/mass spectrometry, and concludes with the applications of GC/MS.

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.

Atomic absorption spectrometry (AAS) is generally used for measuring relatively low concentrations of approximately 70 metallic or semimetallic elements in solution samples. This article describes several features that are common to three techniques, namely, AAS, atomic emission spectrometry (AES), and atomic fluorescence spectrometry (AFS). It discusses the reasons for the extreme differences in AAS sensitivities that affect AFS and AES. The article provides information on the advantages and disadvantages of the Smith/Hieftje system and two types of background correction systems, namely, the continuum-source background correction and Zeeman background correction. It also provides a list of applications of conventional AAS equipment, which includes most of the types of samples brought to laboratories for elemental analyses.

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.

Ferromagnetic resonance (FMR) is used in the identification of the magnetic state of materials, the quantitative determination of static magnetic parameters, and the determination of microwave losses. This article describes the theory of ferromagnetic resonance and provides information on reflection spectrometers, microwave spectrometers, and ferromagnetic anti-resonance spectrometers used for measuring FMR. It also discusses the applications of FMR and provides several detailed examples.

Gas analysis by mass spectrometry, or gas mass spectrometry, is a useful analytical tool for investigations performed in controlled atmospheres or in vacuum. This article provides sufficient information to determine if gas mass spectrometry can produce the data required and to determine the type of instrument necessary for a particular application. It discusses the working operations of gas mass spectrometer components, namely, the introduction system, ion sources, mass analyzers, and the ion detector. The article also provides information on resolution of a gas mass spectrometer determined by the width of the source slit and the collector slit. Finally, it describes the instrument set-up for gas mass spectrometry, and shows how to analyze the test results of gas mass spectrometry.

This article describes the principles and applications of Auger electron spectroscopy (AES). It provides information on the instrumentation typically used in the AES, including an electron gun, an electron spectrometer, a secondary electron detector, and an ion gun. The article also describes experimental methods and limitations of the AES, including elemental detection sensitivity, electron beam artifacts, sample charging, spectral peak overlap, high vapor pressure samples, and sputtering artifacts.