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.

After the fault-tree, a failure-cause identification method has identified potential failure causes and the failure analysis team has prepared a failure mode assessment and assignment (FMA&A). The team knows specifically what to search for when examining components and subassemblies from the failed system. There are numerous techniques and technologies available for examining and analyzing components and subassemblies, which are categorized as follows: optical approaches, dimensional inspection and related approaches, nondestructive test approaches, mechanical and environmental approaches, and chemical and composition analysis for assessing material characteristics. This chapter is a detailed account of the working principle and the steps involved in these techniques and technologies.

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 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.

The ultimate goal of the failure analysis process is to find physical evidence that can identify the root cause of the failure. Transmission electron microscopy (TEM) has emerged as a powerful tool to characterize subtle defects. This article discusses the sample preparation procedures based on focused ion beam milling used for TEM sample preparation. It describes the principles behind commonly used imaging modes in semiconductor failure analysis and how these operation modes can be utilized to selectively maximize signal from specific beam-specimen interactions to generate useful information about the defect. Various elemental analysis techniques, namely energy dispersive spectroscopy, electron energy loss spectroscopy, and energy-filtered TEM, are described using examples encountered in failure analysis. The origin of different image contrast mechanisms, their interpretation, and analytical techniques for composition analysis are discussed. The article also provides information on the use of off-axis electron holography technique in failure analysis.

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.

This article introduces procedures an engineer or materials scientist can use to investigate failures. It provides a brief survey of polymer systems and key properties that need to be measured during failure analysis. The article begins with an overview of the problem-solving approach pertinent to structure analysis. This is followed by a review of the characterization of plastics by infrared and nuclear magnetic resonance spectroscopy. The article then provides information on the distribution of molecular weight of an engineering plastic. It further discusses the methods used in thermal analysis, namely differential thermal analysis, thermogravimetric analysis, thermal-mechanical analysis, and dynamic mechanical analysis. The following sections provide details on X-ray diffraction for analyzing crystalline phases and on a minimal scheme for polymer analysis and characterization to assist the design engineer. The article ends with a discussion on the thermal-analytical scheme for analyzing the milligram quantities of polymer samples.

This chapter describes the various phases that form in tool steels, starting from the base of the Fe-C system to the effects of the major alloying elements. The emphasis is on the phases themselves: their chemical compositions, crystal structures, and properties. The chapter also provides general considerations of phases and phase diagrams and the determination of equilibrium phase diagrams. It describes the formation of martensite, characteristics of alloy carbides, and the design of tool steels.

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 article reviews nondestructive and destructive test methods used to characterize welds. The first process of characterization discussed involves information that may be obtained by direct visual inspection and measurement of the weld. An overview of nondestructive evaluation is included that encompasses techniques used to characterize the locations and structure of internal and surface defects, including radiography, ultrasonic testing, and liquid penetrant inspection. The next group of characterization procedures discussed is destructive tests, requiring the removal of specimens from the weld. The third component of weld characterization is the measurement of mechanical and corrosion properties. Following the discussion on the characterization procedures, the second part of this article provides examples of how two particular welds were characterized according to these procedures.

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 presents definitions of terms related to the metallurgy and metallographic study of irons and steels.

This chapters discusses the basic steps in the failure analysis process. It covers examination procedures, selection and preservation of fracture surfaces, macro and microfractography, metallographic analysis, mechanical testing, chemical analysis, and simulated service testing.

This appendix focuses on procedures, techniques, and precautions associated with the investigation and analysis of metallurgical failures that occur in service. It describes the steps of an orderly failure analysis from collecting and examining samples to performing mechanical and nondestructive tests, preparing and examining fractographs and micrographs, determining failure mode, writing the report, and developing follow-up recommendations. It also examines the fundamental mechanisms of failure, why they occur, and how to identify them by their characteristic features.

This article reviews various analytical techniques most commonly used in plastic component failure analysis. The description of the techniques is intended to make the reader familiar with the general principles and benefits of the methodologies. The descriptions of the analytical techniques are supplemented by a series of case studies that include pertinent visual examination results and the corresponding images that aided in the characterization of the failures. The techniques covered include Fourier transform infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The article also discusses various analytical methods used to characterize the molecular weight distribution of a polymeric material. It provides information on a wide range of mechanical tests that are available to evaluate plastics and polymers, covering the various considerations in the selection and use of test methods.