This article provides a detailed account of the concepts of single-crystal x-ray diffraction (XRD). It begins with a historical review of XRD methods, followed by a description of the various factors involved in crystal symmetry. The article then focuses on the phase problem in x-ray structural analysis and validation of the structural model. Some of the factors to be considered for performing experimental procedure are provided. The article presents several examples of applications of single-crystal XRD. The following sections cover the crystallographic problem in terms of structural analysis, software programs for crystal structure solution and refinement, and visualization of crystal structures. The article ends with a discussion on various databases available for single-crystal XRD analysis.

The primary goal of single-crystal x-ray diffraction is to determine crystal structure and the arrangement of atoms in a unit cell. This article discusses the diffraction of light through line gratings and explains the significance of crystal symmetry, space groups, and diffraction intensities. It also addresses phase and crystallographic analysis along with related challenges, and presents several application examples highlighting various experimental 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.

In x-ray diffraction residual stress measurement, the strain in the crystal lattice is measured, and the residual stress producing the strain is calculated, assuming a linear elastic distortion of the crystal lattice. This article provides a detailed account of the plane stress elastic model, and describes the most common methods of x-ray diffraction residual stress measurement, namely, single-angle and two angle techniques. It elaborates the major steps involved in x-ray diffraction residual stress measurement, explaining the possible sources of error in stress measurement. The article also outlines the applications of x-ray diffraction residual stress measurement with examples.

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.

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.

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.

Neutrons are a principal tool for the study of lattice vibrational spectra in materials. This article provides a detailed account of fission and spallation methods of neutron production that are capable of producing sufficient intensity to be useful in neutron scattering research. It describes the instrumentation required for, and advancements made in, neutron powder diffraction. The article further explains the texture and residual stress (macrostresses and microstresses) problems that are analyzed using the neutron powder diffraction method. It also outlines the single-crystal neutron diffraction technique, and provides examples of the applications of neutron diffraction.

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.

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 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.

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.

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 provides a brief introduction to neutron diffraction as well as its state-of-the-art capabilities. The discussion covers the general principles of the neutron, neutron-scattering theory, generation of neutrons, types of incident radiation, and purposes of single-crystal neutron diffraction, powder diffraction, and pair distribution function analysis. The relationship between detector space and reciprocal space are presented. Various factors involved in sample preparation, calibration, and techniques used for analyzing diffraction data are described. The article also presents application examples and possible future developments in neutron diffraction.

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.

This article provides a detailed account of x-ray diffraction (XRD) residual-stress techniques. It begins by describing the principles of XRD stress measurement, followed by a discussion on the most common methods of XRD residual-stress measurement. Some of the procedures required for XRD residual-stress measurement are then presented. The article provides information on measurement of subsurface stress gradients and stress relaxation caused by layer removal. The article concludes with a section on examples of applications of XRD residual-stress measurement that are typical of industrial metallurgical, process development, and failure analysis investigations undertaken at Lambda Research.

Low-energy electron diffraction (LEED) is a technique for investigating the crystallography of surfaces and overlayers adsorbed on surfaces. This article describes the principles of diffraction from surfaces, and elucidates the method of sample preparation to achieve diffraction patterns. The article describes the limitations of surface sensitive electron diffraction and discusses the applications of LEED with examples.

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.

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.