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 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.

New aircraft wing panels extruded from 7075-T6 aluminum exhibited an unusual pattern of circular black interrupted lines, which could not be removed by scouring or light sanding. The panels, subsequent to profiling and machining, were required to be penetrated inspected, shot peened, H2SO4 anodized, and coated with MIL-C-27725 integral fuel tank coating on the rib side. Scanning electron microscopy and microprobe analysis (both conventional energy-dispersive and Auger analyzers) showed that the anodic coating was applied over an improperly cleaned and contaminated surface. The expanding corrosion product had cracked and, in some places, had flaked away the anodized coating. The corrodent had penetrated the base aluminum in the form of subsurface intergranular attack to a depth of 0.035 mm (0.0014 in.). It was recommended that a vapor degreaser be used during cleaning prior to anodizing. A hot inhibited alkaline cleaner was also recommended during cleaning prior to anodizing. The panels should be dichromate sealed after anodizing. The use of deionized water was also recommended during the dichromate sealing operation. In addition, the use of an epoxy primer prior to shipment of the panels was endorsed. Most importantly, surveillance of the anodizing process itself was emphasized.

Cracks, with no other damage, were observed in a niobium alloy (Nb-106) part when it was pulled from several months of protective storage for assembly into a rocket nozzle. SEM views showed the cracks to be intergranular, with contaminant particles on a large number of the grain facets. EDX analysis showed they consisted of niobium and fluorine. Plastic replicas, prepared by standard TEM techniques, were analyzed with selected-area electron diffraction, showing a pattern match for niobium tetrafluoride. Auger analyses showed electron spectra containing peaks representing carbon, oxygen, nitrogen, fluorine, and chlorine. Investigation into the processing history of the part showed the tenacious oxide film formed by the affinity of niobium for oxygen - even when heat treated in a vacuum – was removed with a combination of strong acids: nitric, hydrochloric, hydrofluoric, and lactic, resulting in the contaminants found on the surface. Thus, residues of the cleaning acid on the part had caused SCC during storage, with the tensile stresses necessary to generate SCC assumed to have been residual stresses from the heat treatment. Recommendation was made that more stringent cleaning procedures to remove any trace of the cleaning acids be used.

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.

The causes of cracking of an as-drawn 90-10 cupronickel tube during mechanical working were investigated to determine the source of embrittlement. Embrittlement was sporadic, but when present was typically noted after the first process anneal. Microstructural and chemical analyses were performed on an embrittled section and on a section from a different lot that did not crack during forming. The failed section showed an intergranular fracture path. Examination of the fracture surfaces revealed the presence of tellurium at the grain boundaries. The source of the tellurium was thought to be contamination occurring in the casting process that became concentrated in the recycled skimmings. It was recommended that future material specifications for skimmings and for externally obtained scrap copper include a trace analysis for tellurium.

During a routine inspection on an aircraft assembly line, an airframe attachment bolt was found to be broken. The bolt was one of 12 that attach the lower outboard longeron to the wing carry-through structure. Failure occurred on the right-hand forward bolt in this longeron splice attachment. The bolt was fabricated from PH13-8Mo stainless steel heat treated to have an ultimate tensile strength of 1517 to 1655 MPa (220 to 240 ksi). A water-soluble coolant was used in drilling the bolt hole where this fastener was inserted. Investigation (visual inspection, 265 SEM images, hardness testing, auger emission spectroscopy and secondary imaging spectroscopy, tensile testing, and chemical analysis) supported the conclusion that failure of the attachment bolt was caused by stress corrosion. The source of the corrosive media was the water-soluble coolant used in boring the bolt holes. Recommendations included inspecting for corrosion all the bolts that were installed using the water-soluble coolant at the spliced joint areas, rinsing all machined bolt holes with a noncorrosive agent, and installing new PH13-8Mo stainless steel bolts with a polysulfide wet sealant.

Two 20 MW turbines suffered damage to second-stage blades prematurely. The alloy was determined to be a precipitation-hardening nickel-base superalloy comparable to Udimet 500, Udimet 710, or Rene 77. Typical protective coatings were not found. Test results further showed that the fuel used was not adequate to guarantee the operating life of the blades due to excess sulfur trioxide, carbon, and sodium in the combustion gases, which caused pitting. A molten salt environmental cracking mechanism was also a factor and was enhanced by the working stresses and by the presence of silicon, vanadium, lead, and zinc. A change of fuel was recommended.

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.

The results of a failure analysis of a series of Cr-Mo-V steel turbine studs which had experienced a service lifetime of some 50,000 h are described. It was observed that certain studs suffered complete fracture while others showed significant defects located at the first stress bearing thread. Crack extension was the result of marked creep embrittlement and reverse temper embrittlement (RTE). Selected approaches were examined to assess the effects of RTE on the material toughness of selected studs. It was observed that Auger electron microscopy results which indicated the extent of grain boundary phosphorus segregation exhibited a good relationship with ambient temperature Charpy data. The electrochemical polarization kinetic reactivation, EPR, approach, however, proved disappointing in that the overlapping scatter in the minimum current density, Ir, for an embrittled and a non-embrittled material was such that no clear decision of the toughness properties was possible by this approach. The initial results obtained from small punch testing showed good agreement with other reported data and could be related to the FATT. Indeed, this small punch test, combined with a miniature sample sampling method, represents an attractive approach to the toughness assessment of critical power plant components.

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.

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.

A Lynx helicopter from the Royal Netherlands Navy lost a rotor blade during preparation for take-off. The blade loss was due to failure of a rotor hub arm by fatigue. The arm was integral to the titanium alloy rotor hub. An extensive material based failure analysis covered the hub manufacture, service damage, and estimates of service stresses. There was no evidence for failure due to poor material properties. However, fractographic and fracture mechanics analyses of the service failure, a full scale test failure, and specimen test failures indicated that the service fatigue stress history could have been more severe than anticipated. This possibility was subsequently supported by a separate investigation of the assumed and actual fatigue loads and stresses.

Results of failure analyses of two aircraft crankshafts are described. These crankshafts were forged from AMS 6414 (similar composition to AISI 4340) vacuum arc remelted steels with sulfur contents of 0.003% (low sulfur) and 0.0005% (ultra-low sulfur). A grain boundary sulfide precipitate was caused by overheat of the low sulfur steel, and an incipient melting of grain boundary junctions was caused by overheat of the ultra-low sulfur steel. The precipitates and incipient melting in these two failed crankshafts were observed during the examination. As expected, impact fractures from the low sulfur steel crankshaft contained planar dimpled facets along separated grain boundaries with a small spherical manganese sulfide precipitates within each dimple. In contrast, planar dimpled facets along separated grain boundaries of impact fractures from the ultra-low sulfur crankshaft steel contained a majority of small spherical particles consisting of nitrogen, boron, iron, carbon, and a small amount of oxygen. Some other dimples contained manganese sulfide precipitates. Fatigue samples machined from the ultra-low sulfur steel crankshaft failed internally at planar grain boundary facets. Some of the facets were covered with nitrogen, boron, iron, and carbon film, while other facets were relatively free of such coverage. Results of experimental forging studies defined the times and temperatures required to produce incipient melting overheat and facets at grain boundary junctions of ultra-low sulfur AMS 6414 steels.

Metal-induced embrittlement is a phenomenon in which the ductility or the fracture stress of a solid metal is reduced by surface contact with another metal in either the liquid or solid form. This article summarizes some of the characteristics of liquid-metal- and solid-metal-induced embrittlement. This phenomenon shares many of these characteristics with other modes of environmentally induced cracking, such as hydrogen embrittlement and stress-corrosion cracking. The discussion covers the occurrence, failure analysis, and service failures of the embrittlement. The article also briefly reviews some commercial alloy systems in which liquid-metal-induced embrittlement or solid-metal-induced embrittlement has been documented and describes some examples of cracking due to these phenomena, either in manufacturing or in service.