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 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 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.

Machine vision is a means of simulating the image recognition and analysis capabilities of the human eye/brain system with electronic and electromechanical techniques. This chapter discusses four basic steps in the machine vision process, namely image formation, image preprocessing, image analysis, and image interpretation. Details of the processes involved, equipment used, and the factors to be considered are also presented. In addition, the applications of machine vision are discussed.

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 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.

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 chapter provides guidelines for conducting metallographic evaluations and offers suggestions on how to effectively report the results. It explains how the approach depends on the objective of the evaluation, which is usually to measure a structural feature, test a hypothesis, or investigate structure-related effects. The chapter addresses each case, tailoring its guidelines and suggestions accordingly.

This chapter describes three approaches for 3D hot-spot localization of thermally active defects by lock-in thermography (LIT). In the first section, phase-shift analysis for analyzing stacked die packages is performed. The second example employs defocusing sequences for the localization of resistive electrical shorts in 3D architectures, and the third operates in cross sectional LIT mode to investigate defects in the insulation liner of Through Silicon Vias. All three approaches allow for a precise localization of thermally active defects in all three spatial dimensions to guide subsequent high-resolution physical analyses.

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 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 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.

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.

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 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.

Magnetic field imaging (MFI), generally understood as mapping the magnetic field of a region or object of interest using magnetic sensors, has been used for fault isolation (FI) in microelectronic circuit failure analysis for almost two decades. Developments in 3D magnetic field analysis have proven the validity of using MFI for 3D FI and 3D current mapping. This article briefly discusses the fundamentals of the technique, paying special attention to critical capabilities like sensitivity and resolution, limitations of the standard technique, sensor requirements and, in particular, the solution to the 3D problem, along with examples of its application to real failures in devices.

Scanning Probe Microscope (SPM) has an increasing important role in the development of nanoscale semiconductor technologies. This article presents a detailed discussion on various SPM techniques including Atomic Force Microscopy (AFM), Scanning Kelvin Probe Microscopy, Scanning Capacitance Microscopy, Scanning Spreading Resistance Microscopy, Conductive-AFM, Magnetic Force Microscopy, Scanning Surface Photo Voltage Microscopy, and Scanning Microwave Impedance Microscopy. An overview of each SPM technique is given along with examples of how each is used in the development of novel technologies, the monitoring of manufacturing processes, and the failure analysis of nanoscale semiconductor devices.

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.