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 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 covers the engineering aspects of corrosion inhibitors and their effect on corrosion reactions. It explains how different metallic salts and heterocyclic compounds influence chemical reactions on metal surfaces exposed to corrosive media or environments. It describes how to evaluate inhibition efficiency through weight loss measurements, linear polarization resistance tests, electrochemical impedance spectroscopy, electrochemical noise monitoring, and surface analysis. It demonstrates the use of potentiodynamic polarization curves, Tafel extrapolations, equivalent circuit models, and various methods for characterizing corrosion damage and protective surface films. It also discusses typical applications, industry trends, and the emerging role of high-throughput experimentation, quantitative modeling, and machine learning in the development of cleaner and more effective corrosion inhibitors.

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 more advanced methods and procedures used in failure analysis, including in-service material sampling, in situ microstructure analysis, and a form of punch testing that can determine the fracture toughness of any material from a tiny specimen. The chapter also covers quantitative fractography, fracture surface topography analysis, and the use of oxide dating as well as fault tree and failure modes and effects analysis (FMEA) and computational techniques.

This article focuses on characterization techniques used for analyzing the physical behavior and chemical composition of thermoset resins, namely chromatography and infrared spectroscopy. The main purpose is to give sufficient detail to permit the reader understand a particular test technique and its value to the thermoset resin field. Epoxy resins are emphasized in the examples because they dominate the airframe and aerospace industries. The article also provides information on two categories of characterization of the processing behavior of thermoset. The first studies the thermal properties of reactive thermoset systems, while the second utilizes these thermal characteristics as the basis for monitoring and control during processing.

Fracture mechanics is a well-developed quantitative approach to the study of failures. This chapter discusses fracture toughness and fracture mechanics, linear-elastic fracture mechanics, and modes of loading. The discussion also covers plane strain and stress and crack growth kinetics. The chapter presents a case history that illustrates the use of fracture mechanics in failure analysis. An appendix provides a more detailed discussion of fracture mechanics concepts.

Forging is a deformation process achieved through the application of compressive stresses. During the stroke, pressures and velocities are continuously changing and the initial lubricant supply must suffice for the duration of the operation. Lubricant residues and pickup products also change with time, further complicating the analysis of friction and wear. This chapter provides a qualitative and quantitative overview of the mechanics and tribology of forging in all of its forms. It discusses the effects of friction, pressures, forces, and temperature on the deformation and flow of metals in open-die, closed-die, and impression-die forging and in back extrusion and piercing operations. It presents various ways to achieve fluid-film lubrication in upset forging processes and examines the cause of barreling, defect formation, and folding in the upsetting of cylinders, rings, and slabs. It also explains how to evaluate lubricants, friction, and wear under hot, cold, and warm forging conditions and how to extend die life and reduce defects when processing different materials.

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.

The relationship of stress and strength gradients must be considered simultaneously in analysis of a particular type of fracture. This chapter discusses the principal elastic stress distribution in members of various shapes under different types of pure loads. A basic understanding of both the stress and strength gradients of metal parts with and without stress concentrations and under different types of loading is provided. The chapter also describes the effect of service conditions on applied stresses.

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 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.

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 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.

Post-mortem analysis of photovoltaic modules that have degraded performance is essential for improving the long term durability of solar energy. This article focuses on a general procedure for analyzing a failed module. The procedure includes electrical characterization followed by thermal imaging such as forward bias, reverse bias, and lock-in, and emission imaging such as electroluminescence and photoluminescence imaging.

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.

The first step in die-level failure analysis is to narrow the search to a specific circuit or transistor group. Then begins the post-isolation process which entails further localizing the defect, determining its electrical, physical, and chemical properties, and examining its microstructure in order to identify the root cause of failure. This chapter assesses the tools and techniques used for those purposes and the challenges brought on by continued transistor scaling, advanced 3D packages, and new IC architectures. The areas covered include sample preparation, nanoprobing, microscopy, FIB circuit edit, and scanning probe microscopy.