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.

Problems with materials compatibility were encountered in pyrotechnically driven devices used in a number of ordnance applications requiring rapid mechanical actuation. A fine bridgewire is located in contact with the chemical pyrotechnic, and the charge is ignited by electrical heating of the bridgewire. Evidence of severe corrosion was revealed on examination of the nickel-chromium-iron alloy bridgewire and the nickel-iron alloy pins. Metallic elements in the pin or bridgewire and substantial amounts of chlorine were detected from the x-ray spectra. Morphological changes indicative of decomposition and dissolution were revealed to have occurred in regions of the pyrotechnic that had been in contact with the bridgewire and pin surfaces by examination of the titanium-potassium perchlorate (Ti-K-Cl-O4) pyrotechnic. Substantial amounts of water were revealed to be associated with the surfaces of the titanium particles in the pyrotechnic by nuclear magnetic resonance. It was proposed that the chlorine-containing residue combined with the water from the pyrotechnic to form a thin aqueous film corroding the bridgewire and pins. A new cleaning procedure was implemented for the glass headers to eliminate the chloride contamination and a vacuum drying procedure was instituted for the pyrotechnic.

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.

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.

A hot rolled, low-carbon steel pot used to melt magnesium alloys leaked, releasing about 35 kg (80 lb) of molten magnesium onto the foundry floor and causing an extensive fire. Due to the fire, the original leakage hole could not be investigated. Samples of the failed pot were polished and etched and were found to be composed of ferrite and pearlite mixtures, as would be expected. However, the sample taken from a location about 75 mm (3 in.) from the hole contained a cluster of unusually large inclusions. By removing the beryllium window from in front of the detector, EPMA spectra were obtained from the inclusions and from the steel matrix. The inclusion spectrum contained primarily iron and oxygen, whereas the matrix spectrum contained primarily iron. X-ray maps were made to show the distribution of iron and oxygen. These results indicated that the inclusions were iron oxide. A similar inclusion at the failure site in the melting pot may have reacted violently with the molten magnesium, causing the leak.

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.

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.

The self-powered flux detectors used in some nuclear reactors are Pt or V-cored co-axial cables with MgO as an insulator and Inconel 600 as the outer sheath material. The detectors are designed to operate in a He atmosphere; to maximize the conduction of heat (generated from the interaction with gamma radiation) and to prevent corrosion. A number of failures have occurred over the years because of a loss of the He cover gas in the assembly. This has resulted in either acid attack on the Inconel 600 sheath in a wet environment or gaseous corrosion in a dry environment. In the latter case, nitriding and embrittlement occurred at temperatures as low as 300 to 400 deg C (determined from an examination of the oxidation of the Zircaloy-2 carrier rod on which the detectors were mounted). Recent results are described and discussed in terms of the oxidation and nitriding kinetics of Zircaloy-2 and Inconel 600, respectively.

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.

Chemical analysis is a critical part of any failure investigation. With the right planning and proper analytical equipment, a myriad of information can be obtained from a sample. This article presents a high-level introduction to techniques often used for chemical analysis during failure analysis. It describes the general considerations for bulk and microscale chemical analysis in failure analysis, the most effective techniques to use for organic or inorganic materials, and examples of using these techniques. The article discusses the processes involved in the chemical analysis of nonmetallics. Advances in chemical analysis methods for failure analysis are also covered.

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 focuses primarily on what an analyst should know about applying X-ray diffraction (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. The article describes the steps required to calibrate instrumentation and to validate stress measurement results. It presents a practical approach to sample selection and specimen preparation, measurement location selection, and measurement depth selection, as well as an outline on measurement validation. The article also provides information on stress-corrosion cracking and corrosion fatigue. The importance of residual stress in fatigue is described with examples. The article explains the effects of heat treatment and manufacturing processes on residual stress. It concludes with a section on the XRD stress measurements in multiphase materials and composites and in locations of stress concentration.

Two investment-cast A356 aluminum alloy actuators used for handles on passenger doors of commercial aircraft fractured during torquing at less than the design load. Visual examination showed that cracking had occurred through a machined side hole. Fractography revealed that the cracks originated in hot tear locations in the castings. Microprobe analysis of fracture surfaces in the hot tear region indicated a much higher silicon-to-aluminum ratio compared with the overload fracture area. No microstructural anomalies related to the failure were found during metallographic examination. It was concluded that the strength of the castings had been compromised by the presence of the casting defects. Modification of the gating system for casting was recommended to eliminate the hot tear zone. It was also suggested that the balance of the castings from the same manufacturing lot be radiographically inspected.

This article focuses on the visual or macroscopic examination of damaged materials and interpretation of damage and fracture features. Analytical tools available for evaluations of corrosion and wear damage features include energy dispersive spectroscopy, electron probe microanalysis, Auger electron spectroscopy, secondary ion mass spectroscopy, and X-ray powder diffraction. The article discusses the analysis and interpretation of base material composition and microstructures. Preparation and examination of metallographic specimens in failure analysis are also discussed. The article concludes with a review of the evaluation of polymers and ceramic materials in failure analysis.

Examination of a damaged component involves a chain of activities that, first and foremost, requires good observation and documentation. Following receipt and documentation, the features of damage can be recorded and their cause(s) investigated, as this article briefly describes, for typical types of damage experienced for metallic components. This article discusses the processes involved in visual or macroscopic examination of damaged material; the interpretation of fracture features, corrosion, and wear damage features; and the analysis of base material composition. It covers the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed.

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.

Although a precise understanding of roll failure genesis is complex, the microstructure of a broken roll can often unravel intrinsic deficiencies in material quality responsible for its failure. This is especially relevant in circumstances when, even under a similar mill-operating environment, the failure involves a particular roll or a specific batch of rolls. This paper provides a microstructural insight into the cause of premature breakage of a second-intermediate Sendzimir mill drive roll used at a stainless steel sheet rolling plant under the Steel Authority of India Limited. Microstructural issues influencing roll quality, such as characteristics of carbides, tempered martensite, retained austenite, etc., have been extensively studied through optical and scanning electron microscopy, electron-probe microanalysis, image analysis, and x-ray diffractometry. These are discussed to elucidate specific microstructural inadequacies that accentuated the failure. The study reveals that even through retained austenite content is low (6.29 vol%) and martensite is non-acicular, the roll breakage is a consequence of intergranular cracking caused by improper carbide morphology and distribution.

An Incoloy 800H (UNS N08810) transfer line on the outlet of an ethane-cracking furnace failed during decoking of the furnace tubes after nine years in service. A metallographic examination using optical and scanning electron microscopy as well as energy-dispersive x-ray spectroscopy revealed that the failure was due to sulfidation. The source of the sulfur in the furnace effluent was either dimethyl disulfide, injected into the furnace feed to prevent coke formation and carburization of the furnace tubes, or contamination of the feed with sulfur bearing oil.

This article is a compilation of abbreviations of terms, techniques, standards, compounds, and properties of materials that are relevant to the characterization and failure analysis of plastics.

A forged 4140 steel shaft that connected two runners in a hydroturbine failed catastrophically after approximately 5900 h of service. The runner and the mating section of the broken shaft were examined and tested by various methods. The results of the analyses indicated that the shaft failed by torsional fatigue starting at subsurface crack initiation sites. The forging contained regions of crack like flaws associated with particles rich in chromium, manganese, and iron. Fracture features indicated that the fatigue cracks propagated under a relatively low stress.