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.

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 provides a detailed account of extended x-ray absorption fine structure (EXAFS). It begins with a description of the fundamentals of EXAFS, providing information on the physical mechanism, single-scattering approximation, and multiple-scattering effects. This is followed by a discussion on the use of synchrotron radiation as an X-ray source for EXAFS. Data-reduction procedures used to extract EXAFS signals are then described. The article also provides information on the analysis of x-ray absorption near-edge structure spectrum and ends with a discussion on the unique features and applications of EXAFS.

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

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

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.

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.

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 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 extended x-ray absorption fine structure (EXAFS). It describes the fundamentals of EXAFS with an emphasis on the physical mechanism, the single-scattering approximation, and multiple-scattering effects. The article discusses the use of synchrotron radiation as the x-ray source for EXAFS experiments. It also describes the typical EXAFS data analysis of pure nickel at 90 K, and explains the near-edge structure analysis of vanadium. The article presents a discussion on the unique features and applications of EXAFS.