A stamped coin exhibited visible discolored areas, seen as a tan haze on the surface. The discoloration was considered merely cosmetic. The nonstained and stained regions were studied using SEM/EDS. Greater amounts of aluminum and magnesium were found in the stained area as compared with the nonstained region. Some carbon and oxygen were detected in both areas, which may be suggestive of organic substances. Fourier transform infrared spectroscopy (FTIR) revealed traces of hydrocarbons and ether/alcohol materials in the stained area, suggesting that the stain was associated with a cellulose or carbohydrates (sugars). These findings, along with the appearance, suggest that a sugar-containing substance, such as coffee or a soft drink, dried onto the surface of this coin and caused the observed discoloration.

A large number of electropolished copper parts showed evidence of discoloration (tinting) after electropolishing. Because these parts are used in a high-vacuum application, even trace amounts of organic materials would be problematic. Scanning electron microscopy of nondiscolored and discolored areas both showed trace amounts of residue in the form of adherent deposits. EDS, FTIR spectroscopy, XPS, and secondary ion mass spectroscopy (SIMS) analyses indicated that the discoloration to the copper components was due to the development of CuO at localized regions. It was recommended that process changes be made to completely remove residual processing fluids from the part surfaces before electropolishing. The use of more aggressive detergents was suggested, and it was recommended also that a filtering and recirculating system be considered for use in the cleaning and electropolishing tanks.

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.

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.

This article presents tools, techniques, and procedures that engineers and material scientists can use to investigate plastic part failures. It also provides a brief survey of polymer systems and the key properties that need to be measured during failure analysis. It describes the characterization of plastics by infrared and nuclear magnetic resonance spectroscopy, differential scanning calorimetry, differential thermal analysis, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The article also discusses the use of X-ray diffraction for analyzing crystal phases and structures in solid materials.

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.

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 reviews analytical techniques that are most often used in plastic component failure analysis. The description of the techniques is intended to familiarize the reader with the general principles and benefits of the methodologies, namely Fourier transform infrared spectroscopy, energy-dispersive x-ray spectroscopy, differential scanning calorimetry, thermogravimetric analysis, and dynamic mechanical analysis. The article describes the methods for molecular weight assessment and mechanical testing to evaluate plastics and polymers. The descriptions of the analytical techniques are supplemented by a series of case studies to illustrate the significance of each method. The case studies also include pertinent visual examination results and the corresponding images that aided in the characterization of the failures.

Grate bars in the traveling grate indurators in several taconite processing units suffered excessive corrosion following a conversion from acid to fluxed pellet production procedures. The campaign life of the HH grade cast stainless steel bars was reduced from more than 7 years to approximately 9 months. Several corroded grate bars were examined metallographically and by electron microscopy to determine the causes of the accelerated corrosion. Chemical and X-ray diffraction analyses were also conducted, along with simulation tests to assess the role of alkali chlorides in the corrosion process. The basic cause of degradation was found to be hot corrosion caused by the deposition of alkali sulfates and chlorides. However this degradation may have been aggravated by thermal cycling and abrasion. The source of the salt was impurities in the flux. Two potential solutions were proposed: modification of the processing parameters to reduce the salt deposition and / or change of bar materials to a more resistant alloy.

A cylindrical spiral gear, part of a locomotive axle assembly, cracked ten days after it had been press-fit onto a shaft, after which it sat in place as other repairs were made. Workers at the locomotive shop reported hearing a sound, and upon inspecting the gear, found a crack extending radially from the bore to the surface of one of the tooth flanks. The crack runs the entire width of the bore, passing through an oil hole in the hub, across the spoke plate and out to the tip of one of the teeth. Design requirements call for the gear teeth to be carburized, while the remaining surfaces, protected by an anti-carburizing coating, stay unchanged. Based on extensive testing, including metallographic examination, microstructural analysis, microhardness testing, and spectroscopy, the oil hole was not protected as required, evidenced by the presence of a case layer. This oversight combined with the observation of intergranular fracture surfaces and the presence of secondary microcracks in the case layer point to hydrogen embrittlement as the primary cause of failure. It is likely that hydrogen absorption occurred during the gas carburizing process.

This article describes the processes involved in photochemical aging and weathering of polymeric materials. It explains how solar radiation, especially in the UV range, combines with atmospheric oxygen, driving photooxidation and the development of unstable photoproducts that cause various types of damage when they decompose, including the scission of carbon bonds and polymer chains. The article illustrates some of the degradation reactions that occur in different polymers and presents an overview of the strategies used to prevent such reactions or otherwise mitigate their effects.

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.

Hydrogen damage is a term used to designate a number of processes in metals by which the load-carrying capacity of the metal is reduced due to the presence of hydrogen. This article introduces the general forms of hydrogen damage and provides an overview of the different types of hydrogen damage in all the major commercial alloy systems. It covers the broader topic of hydrogen damage, which can be quite complex and technical in nature. The article focuses on failure analysis where hydrogen embrittlement of a steel component is suspected. It provides practical advice for the failure analysis practitioner or for someone who is contemplating procurement of a cost-effective failure analysis of commodity-grade components suspected of hydrogen embrittlement. Some prevention strategies for design and manufacturing problem-induced hydrogen embrittlement are also provided.

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.

This article provides an overview of the classification of hydrogen damage. Some specific types of the damage are hydrogen embrittlement, hydrogen-induced blistering, cracking from precipitation of internal hydrogen, hydrogen attack, and cracking from hydride formation. The article focuses on the types of hydrogen embrittlement that occur in all the major commercial metal and alloy systems, including stainless steels, nickel-base alloys, aluminum and aluminum alloys, titanium and titanium alloys, copper and copper alloys, and transition and refractory metals. The specific types of hydrogen embrittlement discussed include internal reversible hydrogen embrittlement, hydrogen environment embrittlement, and hydrogen reaction embrittlement. The article describes preservice and early-service fractures of commodity-grade steel components suspected of hydrogen embrittlement. Some prevention strategies for design and manufacturing problem-induced hydrogen embrittlement are also reviewed.

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.

The cause of the fatigue failure in the retaining ring of the compressor region of an aero-engine turbine was found to be the presence of a high concentration of nonmetallic inclusions. The results of chemical analysis were used to estimate the phases present. The most frequently observed inclusions were spinel solid solutions of the type MO middot; N2O3, where M = Fe, Mn, or Mg and N = Cr or Al. The detrimental inclusions were corundum, calcium aluminates, cristobalite, and silicates. The most detrimental phases were traced on the surfaces of the specimens fractured using impact loading; the comparison is being made with the polished surfaces and the tensile specimen fracture surfaces. The inclusions in the failed retaining ring were compared with the ones in a similar component obtained from a used engine. In the case of the latter, a large number of fine and elongated (Mn, Cr, Fe)S inclusions were present along with spinels. The nondeformable, rigid oxide particles are considered more undesirable than the sulfides as far as fatigue life of the component is concerned. It has been reported that the presence of sulfides may eliminate the stresses due to oxides.

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 briefly reviews the various metallurgical or environmental factors that cause a weakening of the grain boundaries and, in turn, influence the occurrence of intergranular (IG) fractures. It discusses the mechanisms of IG fractures, including the dimpled IG fracture, the IG brittle fracture, and the IG fatigue fracture. The article describes some typical embrittlement mechanisms that cause the IG fracture of steels.

With any polymeric material, chemical exposure may have one or more different effects. Some chemicals act as plasticizers, changing the polymer from one that is hard, stiff, and brittle to one which is softer, more flexible, and sometimes tougher. Often these chemicals can dissolve the polymer if they are present in large enough quantity and if the polymer is not crosslinked. Other chemicals can induce environmental stress cracking (ESC), an effect in which brittle fracture of a polymer will occur at a level of stress well below that required to cause failure in the absence of the ESC reagent. Finally, there are some chemicals that cause actual degradation of the polymer, breaking the macromolecular chains, reducing molecular weight, and diminishing polymer properties as a result. This article examines each of these effects. The discussion also covers the effects of surface embrittlement and temperature on polymer performance.