The overall chemical composition of metals and alloys is most commonly determined by X-ray fluorescence (XRF) and optical emission spectroscopy (OES), and combustion and inert gas fusion analysis. This article provides information on the capabilities, uses, detection threshold and precision methods, and sample requirements. The amount of material that needs to be sampled, operating principles, and limitations of the stated methods are also discussed.

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.

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 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.

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 provides a general introduction of materials characterization and describes the principles and applications of a limited number of techniques that are most commonly used to characterize the composition and structure of metals used in engineering systems. It briefly describes the classification of materials characterization methods including, bulk elemental characterization, bulk structural characterization, microstructural characterization, and surface characterization. Further, the article reviews the selection of materials characterization methods most commonly used with metals.

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.

This article is a compilation of abbreviations, symbols, and tradenames for terms related to the properties, selection, processing, and applications of the most widely used nonmetallic engineering materials.

Coatings and thin films can be studied with surface analysis methods because their inherently small depth allows characterization of the surface composition, interface composition, and in-depth distribution of composition. This article describes principles and examples of common surface analysis methods, namely, Auger electron spectroscopy, X-ray photoelectron spectroscopy, ion scattering spectroscopy, secondary ion mass spectroscopy, and Rutherford backscattering spectroscopy. It also provides useful information on the applications of surface 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.

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.

Quality control of cemented carbides includes the evaluation of physical and chemical properties of constituent raw material powders, powder blends/formulations, green compacts, and fully dense finished product. This article provides a summary of the underlying principles and size ranges for the American Society for Testing and Materials (ASTM) standard methods of particle sizing and distribution. It presents the methods used to analyze the chemical composition of cemented carbide materials in a tabular form. The article also presents information on microstructural evaluation and physical and mechanical property evaluation of cemented carbides.

X-ray diffraction (XRD) is the most extensively used method for identifying and characterizing various aspects of metals related to the arrangements and spacings of their atoms for bulk structural analysis. XRD techniques are also applicable to ceramics, geologic materials, and most inorganic chemical compounds. This article describes the operating principles and types of XRD analyses, along with information about the threshold sensitivity and precision, limitations, sample requirements, and capabilities of related techniques. The necessary instrumentation for XRD analyses include the Debye-Scherrer camera and the X-ray diffractometer. The article also describes the uses of XRD analyses, such as the identification of phases or compounds in metals and ceramics; detection of order and disorder transformation; determination of lattice parameters and changes in lattice parameters due to alloying and temperature effects; measurement of residual stresses; characterization of crystallite size and perfection; characterization of preferred orientations; and determination of single crystal orientations.