This chapter covers the emerging practice of quantitative microscopy and its application in the study of the microstructure of metals. It describes the methods used to quantify structural gradients, volume fraction, grain size and distribution, and other features of interest. It provides examples showing how the various features appear, how they are measured, and how the resulting data are converted into usable form. The chapter also discusses the quantification of fracture morphology and its correlation with material properties and behaviors.

This chapter discusses the context in which metallography is used and some of the challenges of analyzing three-dimensional structures from a two-dimensional perspective. It describes the hierarchical nature of metals, the formation of grain boundaries, and the notable characteristics of microstructure. It explains how microstructure can be represented qualitatively by points, lines, surfaces, and volumes associated to a large extent with grain contact, and how qualitative features (including grains) can be quantified based on cross-sectional area, volume fraction, density, distribution, and other such metrics.

This chapter provides an overview of the tools and techniques used to examine failure specimens and the wealth of information that can be obtained from fracture surfaces, cracks, wear patterns, and other such features. It discusses the use of metallography, fractography, and optical and electron microscopy. It presents a number of images recorded using these methods and explains what they reveal about the mode of fracture and the state of the component prior to failure.

Several specialized instruments are available for the metallographer to use as tools to gather key information on the characteristics of the microstructure being analyzed. These include microscopes that use electrons as a source of illumination instead of light and x-ray diffraction equipment. This chapter describes how these instruments can be used to gather important information about a microstructure. The instruments covered include image analyzers, transmission electron microscopes, scanning electron microscopes, electron probe microanalyzers, scanning transmission electron microscopes, x-ray diffractometers, microhardness testers, and hot microhardness testers. A list of other instruments that are usually located in a research laboratory or specialized testing laboratory is also provided.

This chapter describes some of the most effective tools for investigating boiler tube failures, including scanning electron microscopy, optical emission spectroscopy, atomic absorption spectroscopy, x-ray fluorescence spectroscopy, x-ray diffraction, and x-ray photoelectron spectroscopy. It explains how the tools work and what they reveal. It also covers the topic of image analysis and its application in the measurement of grain size, phase/volume fraction, delta ferrite and retained austenite, inclusion rating, depth of carburization/decarburization, scale thickness, pearlite banding, microhardness, and hardness profiles. The chapter concludes with a brief discussion on the effect of scaling and deposition and how to measure it.

The overall chemical composition of metals and alloys is most commonly determined by x-ray fluorescence (XRF) and optical emission spectroscopy (OES). High-temperature combustion and inert gas fusion methods are typically used to analyze dissolved gases (oxygen, nitrogen, and hydrogen) and, in some cases, carbon and sulfur in metals. This chapter discusses the operating principles of XRF, OES, combustion and inert gas fusion analysis, surface analysis, and scanning auger microprobe analysis. The details of equipment set-up used for chemical composition analysis as well as the capabilities of related techniques of these methods are also covered.

This chapter discusses the techniques applicable to the diagnosis of corrosion failures, including visual and microscopic examination of corroded surfaces and microstructure; chemical analysis of the metal, corrosion products, and bulk environment; nondestructive evaluation methods; corrosion testing techniques; and mechanical testing techniques. A guide to investigative techniques used in corrosion failure analysis is provided in a table, describing the advantages and limitations of each technique. The principal stages of the investigation and analysis of corrosion failures discussed in the chapter are: collection of background information and sampling; preliminary laboratory examination; detailed metallographic and fractographic examinations; chemical analysis of corrosion products and bulk materials; corrosion testing for quality control; mechanical testing for quality control; and analysis of results and report writing.

This chapter elucidates the indispensable role of characterization in the development of cold-sprayed coatings and illustrates some of the common processes used during coatings development. Emphasis is placed on the advanced microstructural characterization techniques that are used in high-pressure cold spray coating characterization, including residual-stress characterization. The chapter includes some preliminary screening of tool hardness and bond adhesion strength, as well as a distinction between surface and bulk characterization techniques and their importance for cold spray coatings. The techniques covered are optical microscopy, X-Ray diffraction, scanning electron microscopy, focused ion beam machining, electron probe microanalysis, transmission electron microscopy, and electron backscattered diffraction. The techniques also include electron channeling contrast imaging, X-Ray photoelectron spectroscopy, X-ray fluorescence, Auger electron spectroscopy, Raman spectroscopy, oxygen analysis, and nanoindentation.

This chapter discusses some of the methods and measurements used to construct phase diagrams. It explains how cooling curves were widely used to determine phase boundaries, and how equilibrated alloys examined under controlled heating and cooling provide information for constructing isothermal and vertical sections as well as liquid projections. It also explains how diffusion couples provide a window into local equilibria and identifies typical phase diagram construction errors along with problems stemming from phase-boundary curvatures and congruent transformations.

Photon emission (PE) is one of the major optical techniques for contactless isolation of functional faults in integrated circuits (ICs) in full electrical operation. This article describes the fundamental mechanisms of PE in silicon based ICs. It presents the opportunities of contactless characterization for the most important electronic device, the MOS - Field Effect Transistor, the heart of ICs and their basic digital element, the CMOS inverter. The article discusses the specification and selection of detectors for proper PE applications. The main topics are image resolution, sensitivity, and spectral range of the detectors. The article also discusses the value and application of spectral information in the PE signal. It describes state of the art IC technologies. Finally, the article discusses the applications of PE in ICs and also I/O devices, integrated bipolar transistors in BiCMOS technologies, and parasitic bipolar effects like latch up.

This chapter discusses the use of electron microscopy in metallographic analysis. It explains how electrons interact with metals and how these interactions can be harnessed to produce two- and three-dimensional images of metal surfaces and generate crystallographic and compositional data as well. It discusses the basic design and operating principles of scanning electron microscopes, transmission electron microscopes, and scanning transmission electron microscopes and how they are typically used. It describes the additional information contained in backscattered electrons and emitted x-rays and the methods used to access it, namely wavelength and energy dispersive spectroscopy and electron backscattering diffraction techniques. It also describes the role of focused ion beam milling in sample preparation and provides information on atom probes, atomic force microscopes, and laser scanning microscopes.

This article covers common techniques for surface characterization, including the modern scanning electron microscopy and methods for the chemical characterization of surfaces by Auger electron spectroscopy, X-ray photoelectron spectroscopy, and time-of-flight secondary ion mass spectrometry. The principles of surface analysis and some of the applications of the technique in polymer failure studies are also provided.

This chapter describes the effects that can be observed by light microscopy when a steel in the hardened condition, consisting of martensite and possibly some retained austenite, is heated at subcritical temperatures. It includes micrographs that illustrate the effect of carbide precipitation, the decomposition of retained austenite, and recovery and recrystallization. It also includes images that reveal the characteristic structures produced by tempering medium-carbon hypoeutectoid and hypereutectoid steels as well as the effects of plastic deformation, austenitic grain size, and temper brittleness.

This chapter explains how the presence of intermediate phases affects the melting behavior of binary alloys and the transformations that occur under different rates of cooling. It begins by examining the phase diagrams of magnesium-lead and copper-zinc, noting some of the complexities associated with intermediate phases. It then discusses the difference between ordered and disordered phases and how they are accounted for on phase diagrams. It describes how the atoms in a disordered solution may arrange themselves into an ordered array, forming a superlattice in the process of cooling, and goes on to identify the most common superlattice structures and their corresponding alloy phases. It also discusses the factors that limit the formation of superlattices along with the kinetics of spinodal decomposition and its effect on microstructure development.

This chapter covers the early studies and various discoveries by metals researchers to study the internal structure of metals. The topics covered include light microscopy, phase diagrams, X-ray diffraction, principles of precipitation hardening, and dislocation theory.

In embedded systems, the separation between system level, board level, and individual component level failure analysis is slowly disappearing. In order to localize the initial defect area, prepare the sample for root cause analysis, and image the exact root cause, the overall functionality has to be maintained during the process. This leads to the requirement of adding additional techniques that help isolate and image defects that are buried deeply within the board structure. This article demonstrates an approach of advanced board level failure analysis by using several non-destructive localization techniques. The techniques considered for advanced fault isolation are magnetic current imaging for shorts and opens; infrared thermography for electrical shorts; time-domain-reflectometry for shorts and opens; scanning acoustic microscopy; and 2D/3D X-Ray microscopy. The individual methods and their operational principles are introduced along with case studies that will show the value of using them on board level defect analysis.

This chapter discusses the important role of metallography and the metallographer in predicting and understanding the properties of metals and alloys. Examples are presented of a metallographer working as part of a team in a research laboratory of a large steel company and a metallographer working alone at a small iron foundry. The three basic areas in all metallography laboratories are discussed: the specimen preparation area, the polishing/etching area, and the observation/micrography area. Important safety issues in a metallographic laboratory are also considered.

This chapter discusses the tools and techniques of light microscopy and how they are used in the study of materials. It reviews the basic physics of light, the inner workings of light microscopes, and the relationship between resolution and depth of field. It explains the difference between amplitude and optical-phase features and how they are revealed using appropriate illumination methods. It compares images obtained using bright field and dark field illumination, polarized and cross-polarized light, and interference-contrast techniques. It also discusses the use of photometers, provides best practices and recommendations for photographing structures and features of interest, and describes the capabilities of hot-stage and hot-cell microscopes.