Thermomechanical analysis (TMA) is a thermal analysis technique in which the length of a specimen is precisely measured versus temperature and time as the specimen is subjected to controlled heating and cooling. This article discusses the various factors and processes involved in TMA. The discussion covers the general principles, equipment used, specimen preparation process, calibration conditions, data analysis steps, and examples of the applications and interpretation of TMA.

This article focuses on the principles and applications of X-ray photoelectron spectroscopy (XPS) for the analysis of elemental and chemical composition. The discussion covers the nomenclature, instruments, and specimen preparation process of XPS. Some of the factors pertinent to the calibration of materials for accurate measurements using XPS are provided, along with some aspects of the accuracy in quantitative analysis by XPS. In addition, the article presents examples of how XPS data can be used to solve problems with surface interactions.

This article reviews many commonly used stereological counting measurements and the relationships based on these parameters. The discussion covers the processes involved in sampling and specimen preparation. Quantitative microstructural measurements are described including volume fraction, number per unit area, intersections and intercepts per unit length, grain size, and inclusion content.

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 detailed information on the instrumentation and principles of the scanning electron microscope (SEM). It begins with a description of the primary components of a conventional SEM instrument. This is followed by a discussion on the advantages and disadvantages of the SEM compared with other common microscopy and microanalysis techniques. The following sections cover the critical issues regarding sample preparation, the physical principles regarding electron beam-sample interaction, and the mechanisms for many types of image contrast. The article also presents the details of SEM-based techniques and specialized SEM instruments. It ends with example applications of various SEM modes.

The reflected light microscope is the most commonly used tool to study the microstructure of metals, composites, ceramics, minerals, and polymers. For the study of the microstructure of metals and alloys, light microscopy is employed in the reflected-light mode using either bright-field illumination, dark-field illumination, polarized light illumination, or differential interference contract, generally by the Nomarski technique. This article concentrates on how to reveal microstructure properly to enable the proper identification of the phases and constituents and, if needed, measuring the amount, size, and spacing of constituents, using the light optical microscope. The discussion covers the examination of microstructures using different illumination methods and includes a comparison between light optical images and scanning electron microscopy images of microstructure.

The electron backscatter diffraction (EBSD) technique has proven to be very useful in the measurement of crystallographic textures, orientation relationships between phases, and both plastic and elastic strains. This article focuses on backscatter diffraction in a scanning electron microscope and describes transmission Kikuchi diffraction. It begins with a discussion on the origins of EBSD and the collection of EBSD patterns. This is followed by sections providing information on EBSD spatial resolution and system operation of EBSD. Various factors pertinent to perform an EBSD experiment are then covered. The article further describes the processes involved in sample preparation that are critical to the success or usefulness of an EBSD experiment. It also discusses the applications of EBSD to bulk samples and the development of EBSD indexing methods.

This article discusses the basic principles of and chemical effects in Auger electron spectroscopy (AES), covering various factors affecting the quantitative analyses of AES. The discussion covers instrumentation and sophisticated electronics typically used in AES for data acquisition and manipulation and various limitations of AES. Various examples highlighting the capabilities of the technique are also included.

This article describes the methods and equipments involved in the preparation of specimens for examination by light optical microscopy, scanning electron microscopy, electron microprobe analysis for microindentation hardness testing, and for quantification of microstructural parameters, either manually or by the use of image analyzers. Preparation of metallographic specimens generally requires five major operations: sectioning, mounting, grinding, chemical polishing, and etching. The article provides information on the principles of technique selection in mechanical polishing, and describes the procedures, advantages, and disadvantages of electrolytic and chemical polishing. It also provides a detailed account of procedures, precautions, and composition for preparation and handling of etchants.

This article describes the metallographic technique for nonferrous metals and special-purpose alloys. These include aluminum alloys, copper and copper alloys, lead and lead alloys, magnesium alloys, nickel and nickel alloys, magnetic alloys, tin and tin alloys, titanium and titanium alloys, refractory metals and alloys, zinc and zinc alloys, and wrought heat-resisting alloys. The preparation of specimens for metallographic technique includes operations such as sectioning, mounting, grinding, polishing, and etching of nonferrous metals and alloys. The article contains tables that list the etchants for macroscopic examination and microscopic examination of nonferrous metals and special-purpose alloys.

Proper sectioning of the surface to be examined is a very important step in preparing steel specimens. The first step in preventing damage to the metallurgical structure is to minimize the amount of sectioning that is done. This article discusses the various metallographic techniques, namely mounting, grinding, polishing, and etching involved in the microstructural analysis of carbon and alloy steels, case hardening steels, cast iron, ferrous powder metallurgy alloys, wrought and cast stainless steels, tool materials, steel castings, iron-chromium-nickel heat-resistant casting alloys and different product forms of steels.

Fractography is the systematic study of fractures and fracture surfaces. It is a useful tool in failure analysis and provides a means for correlating the influence of microstructure on the fracture mode of a given material. This article discusses the preservation, preparation, and photography of fractured parts and surfaces, and describes some of the more common fractographic features revealed by light microscopy, including tensile-fracture surface marks in unnotched specimens, fatigue marks, and structural discontinuities within the metal. The article also explains how to interpret fracture information contained in optical and scanning-electron microscope fractographs.

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 presents examples of the visual fracture examination that illustrate the procedure as it applies to failure analysis and quality determination. It describes the techniques and procedures for the visual and light microscopic examination of fracture surfaces with illustrations. The article also describes microscopic and macroscopic features of the different fracture mechanisms with illustrations with emphasis on visual and light microscopy examination. The types of fractures considered include ductile fractures, tensile-test fractures, brittle fractures, fatigue fractures, and high-temperature fractures.

The application of transmission electron microscope to the study of fracture surfaces and related phenomena has made it possible to obtain magnifications and depths of field much greater than those possible with light (optical) microscopes. This article reviews the methods for preparing single-stage, double-stage, and extraction replicas of fracture surfaces. It discusses the types of artifacts and their effects on these replicas, and provides information on shadowing of replicas. The article concludes with a comparison of the transmission electron and scanning electron fractographs with illustrations.

Plastic deformation can occur in metals from various mechanisms, such as slip, twinning, diffusion creep, grain-boundary sliding, grain rotation, and deformation-induced phase transformations. This article emphasizes on the mechanism of slip and twinning under cold working conditions. It discusses the factors on which the structures developed during plastic deformation depend. These factors include crystal structure, amount of deformation, composition, deformation mode, and deformation temperature and rate. The article illustrates the microstructural features that appear after substantial deformation when revealed through metallographic investigation.

This article is an atlas of fractographs that covers nickel-base superalloys. The fractographs display the following: hydrogen-embrittlement fracture; segment of a fractured second-stage gas-turbine wheel; gas-producer turbine rotor cast; dendritic stress-rupture fracture surface; fatigue and creep fractures; simultaneous metallographic-fractographic evaluation; and effect of thermal cycling on fatigue fracture.

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.

Powder forging is an extension of the conventional press and sinter powder metallurgy process, which is recognized as an effective technology for producing a variety of parts to net or near-net shape. This article focuses on the material considerations, such as powder characteristics, alloy development, and inclusion assessment; and process considerations, such as process stages, tool design, and secondary operations; of ferrous alloy powder forging. The mechanical properties of powder forged materials are also reviewed. The article discusses the quality assurance tests for powder forged materials: the part dimensions and surface finish measurement, magnetic particle inspection, metallographic analysis, and nondestructive testing. It concludes with a discussion on the applications of powder forged parts with examples.

Heat treatment of aluminum alloys is assessed by various quality-assurance methods that include metallographic examination, hardness measurements, mechanical property tests, corrosion-resistance tests, and electrical conductivity testing. The use of hardness measurements in the quality assurance of heat treated aluminum products is effectively used in conjunction with the measurement of surface electrical conductivity. This article provides a detailed discussion of the error sources in eddy-current conductivity measurements. It also presents useful information on the variation of electrical conductivity of alloy 2024 samples as a function of aging time at different isothermal holding temperatures.