This article covers the three most popular techniques used to characterize the very outermost layers of solid surfaces: Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). Some of the more important attributes are listed for preliminary insight into the strengths and limitations of these techniques for chemical characterization of surfaces. The article describes the basic theory behind each of the different techniques, the types of data produced from each, and some typical applications. Also discussed are the different types of samples that can be analyzed and the special sample-handling procedures that must be implemented when preparing to do failure analysis using these surface-sensitive techniques. Data obtained from different material defects are presented for each of the techniques. The examples presented highlight the typical data sets and strengths of each technique.

This article provides information on the chemical characterization of surfaces by Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). It describes the basic theory behind each of these techniques, the types of data produced from each, and some typical applications. The article explains the strengths of AES, XPS, and TOF-SIMS based on data obtained from the surface of a slightly corroded stainless steel sheet.

The operator of an electric transit system purchased a large number of tin-plated copper connectors, putting some in service and others in reserve. Later, when some of the reserve connectors were inspected, the metal surfaces were covered with spots consisting of an ash-like powder and the plating material had separated from the substrate in many areas. Several connectors, including some that had been in service, were examined to determine what caused the change. The order stated that the connectors were to be coated with a layer of tin-bismuth (2% Bi) to guard against tin pest, a type of degradation that occurs at low temperatures. Based on the results of the investigation, which included SEM/EDS analysis, inductively coupled plasma spectroscopy, and x-ray diffraction, the metal surfaces contained less than 0.1% Bi and thus were not adequately protected against tin pest, which was confirmed as the failure mechanism in the investigation.

Identification of alloys using quantitative chemical analysis is an essential step during a metallurgical failure analysis process. There are several methods available for quantitative analysis of metal alloys, and the analyst should carefully approach selection of the method used. The choice of appropriate analytical techniques is determined by the specific chemical information required, the condition of the sample, and any limitations imposed by interested parties. This article discusses some of the commonly used quantitative chemical analysis techniques for metals. The discussion covers the operating principles, applications, advantages, and disadvantages of optical emission spectroscopy (OES), inductively coupled plasma optical emission spectroscopy (ICP-OES), X-ray spectroscopy, and ion chromatography (IC). In addition, information on combustion analysis and inert gas fusion analysis is provided.

X-ray spectroscopy is generally accepted as the most useful ancillary technique that can be added to any scanning electron microscope (SEM), even to the point of being considered a necessity by most operators. While “stand-alone” x-ray detection systems are used less frequently in failure analysis than the more exact instrumentation employed in SEMs, the technology is advancing and is worthy of note due to its capability for nondestructive analysis and application in the field. This article begins with information on the basis of the x-ray signal. This is followed by information on the operating principles and applications of detectors for x-ray spectroscopy, namely energy-dispersive spectrometers, wavelength-dispersive spectrometers, and handheld x-ray fluorescence systems. The processes involved in x-ray analysis in the SEM and handheld x-ray fluorescence analysis are then covered. The article ends with a discussion on the applications of x-ray spectroscopy in failure analysis.

This article provides an overview of the electrochemical nature of corrosion and analyzes corrosion-related failures. It describes corrosion failure analysis and discusses corrective and preventive approaches to mitigate corrosion-related failures of metals. These include: change in the environment; change in the alloy or heat treatment; change in design; use of galvanic protection; use of inhibitors; use of nonmetallic coatings and liners; application of metallic coatings; use of surface treatments, thermal spray, or other surface modifications; corrosion monitoring; and preventive maintenance.

This article describes some of the common elemental composition analysis methods and explains the concept of referee and economy test methods in failure analysis. It discusses different types of microchemical analyses, including backscattered electron imaging, energy-dispersive spectrometry, and wavelength-dispersive spectrometry. The article concludes with information on specimen handling.

This article provides information on the development of finite element analysis (FEA) and describes the general-purpose applications of FEA software programs in structural and thermal, static and transient, and linear and nonlinear analyses. It discusses special-purpose finite element applications in piping and pressure vessel analysis, impact analysis, and microelectronics. The article describes the steps involved in the design process using the FEA. It concludes with two case histories that involve the use of FEA in failure analysis.

The scanning electron microscopy (SEM) is one of the most versatile instruments for investigating the microstructure of metallic materials. This article highlights the development of SEM technology and describes the operation of basic systems in an SEM, including the electron optical column, signal detection and display equipment, and vacuum system. It discusses the preparation of samples for observation using an SEM and describes the application of SEM in fractography. If the surface remains unaffected and undamaged by events subsequent to the actual failure, it is often a simple matter to determine the failure mode by the use of an SEM. In cases where the surface is altered after the initial failure, the case may not be so straightforward. The article presents typical examples that illustrate these points. Image dependence on the microscope type and operating parameters is also discussed.

The scanning electron microscope (SEM) is one of the most versatile instruments for investigating the microscopic features of most solid materials. The SEM provides the user with an unparalleled ability to observe and quantify the surface of a sample. This article discusses the development of SEM technology and operating principles of basic systems of SEM. The basic systems covered include the electron optical column, signal detection and display equipment, and the vacuum system. The processes involved in the preparation of samples for observation using an SEM are described, and the application of SEM in fractography is discussed. The article covers the failure mechanisms of ductile failure, brittle failure, mixed-mode failure, and fatigue failure. Lastly, image dependence on microscope type and operating parameters is also discussed.

Corrosion is the deterioration of a material by a reaction of that material with its environment. The realization that corrosion control can be profitable has been acknowledged repeatedly by industry, typically following costly business interruptions. This article describes the electrochemical nature of corrosion and provides the typical analysis of environmental- and corrosion-related failures. It presents common methods of testing of laboratory corrosion and discusses the processes involved in the prevention of environmental- and corrosion-related failures of metals and nonmetals.

When complex designs, transient loadings, and nonlinear material behavior must be evaluated, computer-based techniques are used. This is where the finite-element analysis (FEA) is most applicable and provides considerable assistance in design analysis as well as failure analysis. This article provides a general view on the applicability of finite-element modeling in conducting analyses of failed components. It highlights the uses of finite-element modeling in the area of failure analysis and design, with emphasis on structural analysis. The discussion covers the general development and both general- and special-purpose applications of FEA. The special-purpose applications of FEA covered are piping and pressure vessel analysis, impact analysis, and microelectronic and microelectromechanical systems analysis. The article provides case histories that involved the use of FEA in failure analysis.

This article discusses the operating principles, advantages, and limitations of scanning electron microscopy, atomic force microscopy, x-ray photoelectron spectroscopy, and secondary ion mass spectroscopy that are used to analyze the surface chemistry of plastics.

Tribology is the study of contacting materials in relative motion and more specifically the study of friction, wear, and lubrication. This article discusses the classification and the mechanisms of friction, wear, and lubrication of polymers. It describes the tribological applications of polymers and the tribometers and instrumentation used to measure the tribological properties of polymers. The article discusses the processes involved in calculating the wear rate of polymers and the methods of characterization of the sliding interface. It provides information on the pressure and velocity limit of polymer composites and polymer testing best practices.

This article provides practical information and data on property development in engineering plastics. It discusses the effects of composition on submolecular and higher-order structure and the influence of plasticizers, additives, and blowing agents. It examines stress-strain curves corresponding to soft-and-weak, soft-and-tough, hard-and-brittle, and hard-and-tough plastics and temperature-modulus plots representative of polymers with different degrees of crystallinity, cross-linking, and polarity. It explains how viscosity varies with shear rate in polymer melts and how processes align with various regions of the viscosity curve. It discusses the concept of shear sensitivity, the nature of viscoelastic properties, and the electrical, chemical, and optical properties of different plastics. It also reviews plastic processing operations, including extrusion, injection molding, and thermoforming, and addresses related considerations such as melt viscosity and melt strength, crystallization, orientation, die swell, melt fracture, shrinkage, molded-in stress, and polymer degradation.

X-ray diffraction (XRD) residual-stress analysis is an essential tool for failure analysis. This article focuses primarily on what the analyst should know about applying XRD residual-stress measurement techniques to failure analysis. Discussions are extended to the description of ways in which XRD can be applied to the characterization of residual stresses in a component or assembly and to the subsequent evaluation of corrective actions that alter the residual-stress state of a component for the purposes of preventing, minimizing, or eradicating the contribution of residual stress to premature failures. The article presents a practical approach to sample selection and specimen preparation, measurement location selection, and measurement depth selection; measurement validation is outlined as well. A number of case studies and examples are cited. The article also briefly summarizes the theory of XRD analysis and describes advances in equipment capability.

This article discusses the most common thermal analysis methods for thermosetting resins. These include differential scanning calorimetry, thermomechanical analysis, thermogravimetric analysis, and dynamic mechanical analysis. The article also discusses the characterization of uncured thermosetting resins as well as the curing process. Then, the techniques to characterize the physical properties of cured thermosets and composites are presented. Several examples of stress-strain curves are shown for thermosets and thermoplastic polymers.

Nondestructive testing (NDT), also known as nondestructive evaluation (NDE), includes various techniques to characterize materials without damage. This article focuses on the typical NDE techniques that may be considered when conducting a failure investigation. The article begins with discussion about the concept of the probability of detection (POD), on which the statistical reliability of crack detection is based. The coverage includes the various methods of surface inspection, including visual-examination tools, scanning technology in dimensional metrology, and the common methods of detecting surface discontinuities by magnetic-particle inspection, liquid penetrant inspection, and eddy-current testing. The major NDE methods for internal (volumetric) inspection in failure analysis also are described.