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.

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 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 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 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.

As semiconductor feature sizes have shrunk, the technology needed to encapsulate modern integrated circuits has expanded. Due to the various industry changes, package failure analyses are becoming much more challenging; a systematic approach is therefore critical. This article proposes a package failure analysis flow for analyzing open and short failures. The flow begins with a review of data on how the device failed and how it was processed. Next, non-destructive techniques are performed to document the condition of the as-received units. The techniques discussed are external optical inspection, X-ray inspection, scanning acoustic microscopy, infrared (IR) microscopy, and electrical verification. The article discusses various fault isolation techniques to tackle the wide array of failure signatures, namely IR lock-in thermography, magnetic current imaging, time domain reflectometry, and electro-optical terahertz pulse reflectometry. The final step is the step-by-step inspection and deprocessing stage that begins once the defect has been imaged.

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 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.

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 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 article is a compilation of abbreviations and symbols related to characterization and failure analysis of plastics.

There are several analytical methods available that can be used in-line on whole wafers as well as off-line on de-processed products that are returned from the field. These techniques are surface analytical techniques that can be used to characterize the bulk of the material. The main six methods used in semiconductor industry are: Auger spectroscopy, dynamic secondary ion mass spectroscopy, time of flight static secondary ion mass spectroscopy (ToF-SIMS), X-ray photoelectron spectroscopy, scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDX), and transmission electron microscope-EDX. This review specifically addresses ToF-SIMS and describes some typical examples of the application of Auger and SEM-EDX.

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.

Most of the counterfeit parts detected in the electronics industry are either novel or surplus parts or salvaged scrap parts. This article begins by discussing the type of parts used to create counterfeits. It discusses the three most commonly used methods used by counterfeiters to create counterfeits. These include relabeling, refurbishing, and repackaging. The article presents a systematic inspection methodology that can be applied for detecting signs of possible part modifications. The methodology consists of external visual inspection, marking permanency tests, and X-ray inspection followed by material evaluation and characterization. These processes are typically followed by evaluation of the packages to identify defects, degradations, and failure mechanisms that are caused by the processes (e.g., cleaning, solder dipping of leads, reballing) used in creating counterfeit parts.

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 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.