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 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 discusses the effects of corrosion on boiler tube surfaces exposed to water and steam. It describes the process of corrosion, the formation of scale, and the oxides of iron from which it forms. It addresses the primary types of corrosion found in boiler environments, including general corrosion, under-deposit corrosion, microbially induced corrosion, flow-accelerated corrosion, stress-assisted corrosion, erosion-corrosion, cavitation, oxygen pitting, stress-corrosion cracking, and caustic embrittlement. The discussion is supported by several illustrations and relevant case studies.

This appendix defines abbreviations, acronyms, and symbols presented within this book.

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 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.

Fossil fuels produce many byproducts that, if not fully combusted, put boiler tubes at risk. Fuel ash, chemical residues, and process heat pose the greatest threat and are the primary contributors to fireside corrosion. This chapter covers various types of fireside corrosion such as waterwall, fuel ash, and hot corrosion, acid dew-point or cold-end corrosion, and polythionic acid corrosion. It also addresses stress corrosion cracking and includes relevant case studies.

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.

Boiler tubes subjected to cyclic or fluctuating loads over extended periods of time are prone to fatigue failure. Fatigue can occur at relatively low stresses and is implicated in almost 80% of the tube failures in firetube boilers. This chapter covers the most common forms of boiler tube fatigue, including mechanical or vibrational fatigue, corrosion fatigue, thermal fatigue, and creep-fatigue interaction. It discusses the causes, characteristics, and impacts of each type and provides several case studies.

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 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.

Boiler tubes operating at high temperatures under significant pressure are vulnerable to stress rupture failures. This chapter examines the cause, effect, and appearance of such failures. It discusses the conditions and mechanisms that either lead to or are associated with stress rupture, including overheating, high-temperature creep, graphitization, and dissimilar metal welds. It explains how to determine which mechanisms are in play by interpreting fracture patterns and microstructural details. It also describes the investigation of several carbon and low-alloy steel tubes that failed due to stress rupture.

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.

Boiler tube failures associated with material defects are often the result of poor quality control, whether in primary production, on-site fabrication, storage and handling, or installation. This chapter examines quality-related failures stemming from compositional and structural defects, forming and welding defects, design defects, improper cleaning methods, and ineffective maintenance. It also includes case studies and illustrations.

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.