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 article provides an overview of how to use the scanning electron microscope (SEM) for imaging integrated circuits. The discussion covers the principles of operation and practical techniques of the SEM. The techniques include sample mounting, sample preparation, sputter coating, sample tilt and image composition, focus and astigmatism correction, dynamic focus and image correction, raster alignment, and adjusting brightness and contrast. The article also provides information on achieving ultra-high resolution in the SEM. It concludes with information on the general characteristics and applications of environmental SEM.

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 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 chapter provides perspective on the physical dimensions associated with the microstructure of steel and the instruments that reveal grain size, morphology, phase distributions, crystal defects, and chemical composition, from which properties and behaviors derive. The chapter also reviews the definitions and classifications used to identify and differentiate commercial steels, including the AISI/SAE and UNS designation systems.

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 article provides an overview of the most common micro-analytical technique in the failure analysis laboratory: energy dispersive X-ray spectroscopy (EDS). It discusses the general characteristics, advantages, and disadvantages of some of the X-ray detectors attached to the scanning electron microscope chamber including the lithium-drifted EDS detector, silicon drift detector (SDD), and wavelength dispersive X-ray detector. The article then provides information on qualitative and quantitative X-ray analysis programs followed by a discussion on EDS elemental mapping. The discussion includes a comparison of scanning transmission electron microscope-EDS elemental mapping and mapping with an SDD. A brief section is devoted to the discussion on the artifacts that occur during X-ray mapping.

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.

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.

This chapter discusses the principles of scanning transmission electron microscopy (STEM) as implemented using conventional scanning electron microscopes (SEMs). It describes the pros and cons of low-energy imaging and diffraction, addresses basic hardware requirements, and provides information on imaging modes, detector positioning and alignment, and the effect of contrast reversal. It also discusses beam convergence and angular selectivity, the use of application-specific masks, and how to generate grain orientation maps for different material systems.

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 article presents methods that enable one to consistently, uniformly and quickly remove substrate silicon from units without imparting damage to the structure of interest. It provides examples of electron beam probing and backside nano-probing techniques. The electron beam probing techniques are E-beam Logic State Imaging, Electron-beam Signal Image Mapping, and E-beam Device Perturbation. Backside nano-probing techniques discussed include: Electron Beam Absorbed Current, Electron Beam Induced Resistance Change, four terminal resistance measurements, resistive gate defect identification, and circuit editing. The article also presents methods to prepare electron beam probing samples where some remaining silicon is required for the transistor functions and transmission electron microscope samples from units where the substrate silicon has been partially or completely removed.

With the commercialization of heavier and lighter ion beams, adoption of focused ion beam (FIB) use for analysis of challenging regions of interest (ROI) has grown. In this chapter, the authors focus on highlighting commercially available and complementary FIB technologies and their implementation challenges and application trends.

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.

This chapter provides information on ultra-light steel family research programs conducted by the global steel industry under the umbrella of WorldAutoSteel. It discusses the collaboration efforts between U.S government, industry, and academia on advanced high-strength steels (AHSS) technology. Some of the projects on AHSS research and development are also reviewed.

Optoelectronic components can be readily classified as active light-emitting components (such as semiconductor lasers and light emitting diodes), electrically active but non-emitting components, and inactive components. This chapter focuses on the first category, and particularly on semiconductor lasers. The discussion begins with the basics of semiconductor lasers and the material science behind some causes of device failure. It then covers some of the common failure mechanisms, highlighting the need to identify failures as wearout or maverick failures. The chapter also covers the capabilities of many key optoelectronic failure analysis tools. The final section describes the common steps that should be followed so as to assure product reliability of optoelectronic components.

This chapter discusses material-related problems associated with coal-fired burners. It explains how high temperatures affect heat-absorbing surfaces in furnace combustion areas and in the convection pass of superheaters and reheaters. It describes how low-NOx combustion technology, intended to reduce NOx emissions, accelerates tube wall wastage. It also covers circumferential cracking in furnace waterwalls, thermal fatigue cracking induced by waterlances and water cannons, superheater-reheater corrosion, and erosion in fluidized-bed boilers.

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.