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.

Metallographic examination is one of the most important procedures used by metallurgists in failure analysis. Typically, the light microscope (LM) is used to assess the nature of the material microstructure and its influence on the failure mechanism. Microstructural examination can be performed with the scanning electron microscope (SEM) over the same magnification range as the LM, but examination with the latter is more efficient. This article describes the major operations in the preparation of metallographic specimens, namely sectioning, mounting, grinding, polishing, and etching. The influence of microstructures on the failure of a material is discussed and examples of such work are given to illustrate the value of light microscopy. In addition, information on heat-treatment-related failures, fabrication-/machining-related failures, and service failures is provided, with examples created using light microscopy.

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.

Examination of a damaged component involves a chain of activities that, first and foremost, requires good observation and documentation. Following receipt and documentation, the features of damage can be recorded and their cause(s) investigated, as this article briefly describes, for typical types of damage experienced for metallic components. This article discusses the processes involved in visual or macroscopic examination of damaged material; the interpretation of fracture features, corrosion, and wear damage features; and the analysis of base material composition. It covers the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed.

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 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 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.

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.

This article introduces various techniques commonly used in the characterization of semiconductors, namely single-crystal, polycrystalline, amorphous, oxide, organic, and low-dimensional semiconductors and semiconductor devices. The discussion covers material classification, fabrication methods, sample preparation, bulk/elemental characterization methods, microstructural characterization methods, surface characterization methods, and electronic characterization methods.

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 introduces thermal spray coatings and describes the various types of coating processes and coating devices, including the flame spray, electric-arc spray, plasma spray, transferred plasma arc, high-velocity oxyfuel, and detonation gun. It provides information on the surface preparation methods and finishing treatments of coated parts. The article also explains the tests to evaluate the coating quality and the effects of coating structures and mechanical properties on coated parts. It concludes with a discussion on the uses of thermal spray coatings.

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.

Titanium alloys are forged into a variety of shapes and types of forgings, with a broad range of final part forging design criteria based on the intended end-product application. This article begins with a discussion on the classes of titanium alloys, their forgeability, and factors affecting forgeability. It describes the forging techniques, equipment, and common processing elements associated with titanium alloy forging. The processing elements include the preparation of forging stock, preheating of the stock, die heating, lubrication, forging process, trimming and repair, cleaning, heat treatment, and inspection. The article presents a discussion on titanium alloy precision forgings and concludes with information on the forging of advanced titanium materials and titanium aluminides.

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.

Failure analysis is a process that is performed in order to determine the causes or factors that have led to an undesired loss of functionality. This article is intended to demonstrate proper approaches to failure analysis work. The goal of the proper approach is to allow the most useful and relevant information to be obtained. The discussion covers the principles and approaches in failure analysis work, objectives and scopes of failure analysis, the planning stages for failure analysis, the preparation of a protocol for a failure analysis, practices used by failure analysts, and procedures of failure analysis.

Hard chromium plating is produced by electrodeposition from a solution containing chromic acid and a catalytic anion in proper proportion. This article presents the major uses of hard chromium plating, and focuses on the selection factors, plating solutions, solution and process control, equipment, surface preparation, and crack patterns and other characteristics of hard chromium plating. It offers recommendations for the design and use of plating racks, describes the problems encountered in hard chromium plating, and their corrective procedures. The article provides information on the removal of chromium plate from coated metals, recovery and disposal of wastes, and stopoff media for selective plating.

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.

Visual examination, using the unaided eye or a low-power optical magnifier, is typically one of the first steps in a failure investigation. This article presents the guidelines for selecting samples for scanning electron microscope examination and optical metallography and for cleaning fracture surfaces. It discusses damage characterization of metals, covering various factors that influence the damage, namely stress, aggressive environment, temperature, and discontinuities.