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.

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.

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.

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.