This article presents the experimental and theoretical aspects of small-angle scattering, and discusses specific applications used in the characterization of metals, glasses, polymers, and ceramics. The basic methods of collimating x-rays, the cause of smearing from a line source, desmearing parameters, and the types of scattering curves are illustrated.

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.

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.

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 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.

The diffraction pattern of any material contains structural and chemical property information that can be extracted using radial distribution function analysis. This article provides an introduction to the technique and presents several examples highlighting various ways in which it can be used. It begins with a discussion on the principles of diffraction and scattering and the effectiveness of x-ray, neutron, and electron energy sources for different types of measurements. It provides information on data collection and reduction and explains how to create atomic distribution plots from intensity and scattering angle data. The article also presents application parameters for defining short distances and background intensity and describes a procedure for generating pair distribution functions.

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 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.

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 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.

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.

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.

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.

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 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.

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.