X-ray powder diffraction (XRPD) techniques are used to characterize samples in the form of loose powders or aggregates of finely divided material that readily diffract x-rays in specified patterns. This article provides an introduction to XRPD, beginning with a review of sensing devices, including pinhole/Laue cameras, Debye-Scherrer/Gandolfi cameras, Guinier cameras, glancing angle cameras, conventional diffractometers, thin film diffractometers, Guinier diffractometers, and micro diffractometers. The article then describes several quantitative measurement methods, such as lattice parameter, absorption diffraction, spiking, and direct comparison, explaining where each may be used. It also identifies potential sources of error in XRPD measurements.

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.

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 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 describes the structure of coatings produced by plasma spraying, vapor deposition, and electrodeposition processes. The main techniques used for microstructure assessment are introduced. The relationship between the microstructure and property is also discussed. The experimental techniques for microstructural characterization include metallographic technique, X-ray diffraction, electron, microscopies, and porosimetry.

X-ray powder diffraction (XRPD) techniques are used to characterize samples in the form of loose powders, aggregates of finely divided material or polycrystalline specimens. This article provides a detailed account of XRPD. It begins with a discussion on XRPD instrumentation and the techniques used to characterize samples. The article then describes the principles, advantages, and disadvantages of various types of powder diffractometers. A section on the Rietveld method of diffraction analysis is then presented. The article discusses various methods and procedures for qualifying and quantifying phase mixtures in powder samples. It provides information on typical sensitivity and experimental limits on precision of XRPD analysis and other systematic sources of errors that affect accuracy. Some of the factors pertinent to the estimation of crystallite size and defects are also presented. The article ends with a few application examples of XRPD.

Scanning electron microscopy (SEM) has unique capabilities for analyzing fracture surfaces. This article discusses the basic principles and practice of SEM, with an emphasis on its applications in fractography. The topics include an introduction to SEM instrumentation, imaging and analytical capabilities, specimen preparation, and the interpretation of fracture features. SEM can be subdivided into four systems, namely, illuminating/imaging, information, display, and vacuum systems. The article also describes the major criteria and techniques of SEM specimen preparation, and the general features of ductile and brittle fracture modes.

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.

X-ray topography is a technique that comprises topography and x-ray diffraction. This article provides a description of the kinematical theory and the dynamical theory of diffraction. It provides useful information on the configurations of reflection and transmission topography. The article explains various topographic methods, namely, divergent beam method, polycrystal rocking curve analysis, line broadening analysis, microbeam method, and polycrystal scattering topography, as well as their instrumentation. It also describes the applications of x-ray topography.

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 various concepts of micro x-ray diffraction (XRD) used for the examination of materials in situ. The discussion covers the principles, equipment used, sample preparation procedure, considerations for calibrating a detector, steps for performing data analysis, and applications and interpretation of micro-XRD.

X-ray diffraction techniques are useful for characterizing crystalline materials, such as metals, intermetallics, ceramics, minerals, polymers, plastics, and other inorganic or organic compounds. This article discusses the theory of x-rays and how they are generated and detected. It also describes the crystalline nature of certain materials and how the geometry of a unit cell, and hence crystal lattice, affects the direction and intensity of diffracted x-ray beams. The article concludes with several application examples involving measurements on single and polycrystalline materials.

Analytical transmission electron microscopy (ATEM) is unique among materials characterization techniques as it enables essentially the simultaneous examination of microstructural features through high-resolution imaging and the acquisition of chemical and crystallographic information from small regions of the specimen. This article illustrates the effectiveness of the technique in solving materials problems. The first section of the article provides information on analytical electron microscope (AEM) and its basic operational characteristics as well as on electron optics, electron beam/specimen interactions and the generation of a signal, signal detectors, electron diffraction, imaging, x-ray microanalysis, electron energy loss spectroscopy, and sample preparation. The second section consists of 12 examples, each illustrating a specific type of materials problem that can be solved, at least in part, with AEM.

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 topography is the general term for a family of x-ray diffraction imaging techniques capable of providing information on the nature and distribution of imperfections. This article provides a detailed account of x-ray topography techniques, providing information on the historical background and development trends in x-ray diffraction topography. The discussion covers the general principles, components of systems, and applications of x-ray topography techniques, namely conventional X-ray topographic techniques and synchrotron x-ray topographic techniques.

This article discusses the techniques and applications of synchrotron x-ray diffraction, providing information on x-ray generation, monochromation, and crystallography. X-ray diffraction techniques covered include single-crystal and powder diffraction. Some of the factors involved in the construction and development of macromolecular x-ray crystallography are also described.

Metal transparency and interaction with X-rays have been recognized as obvious candidate principles from which methods for in situ monitoring of solidification processes could be developed. This article describes the use of X-ray imaging-based techniques to investigate interface morphology evolution, solute transport, and various process phenomena at spatiotemporal resolutions. It discusses the three viable imaging techniques made available by synchrotron radiation for the real-time investigation of solidification microstructures in alloys. These include two-dimensional X-ray topography, two-dimensional X-ray radiography, and ultra-fast three-dimensional X-ray tomography.

This article describes the methods of X-ray diffraction analysis, the types of information that can be obtained, and its interpretation. The discussion covers the basic theories of X-rays and various types of diffraction experiments, namely single-crystal methods for polychromatic and monochromatic beams, powder diffraction methods, and the Rietveld method.

The scanning electron microscope (SEM) is one of the most versatile instruments for investigating the microscopic features of most solid materials. The SEM provides the user with an unparalleled ability to observe and quantify the surface of a sample. This article discusses the development of SEM technology and operating principles of basic systems of SEM. The basic systems covered include the electron optical column, signal detection and display equipment, and the vacuum system. The processes involved in the preparation of samples for observation using an SEM are described, and the application of SEM in fractography is discussed. The article covers the failure mechanisms of ductile failure, brittle failure, mixed-mode failure, and fatigue failure. Lastly, image dependence on microscope type and operating parameters is also discussed.

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