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.

Accelerated aging tests on detonator assemblies, to verify the compatibility of gold bridgewire and Pd-In-Sn solder with the intended explosives, revealed an unusual form of corrosion. The tests, conducted at 74 deg C (165 deg F) and 54 deg C (130 deg F), indicated a preferential attack of the gold. To investigate the problem, a matrix of test units was produced and analyzed. Scanning electron microscopy, EDX analysis, and x-ray diffraction techniques were used to determine the extent of the corrosion and identify the corrosion products. The results indicated that the preferential attack of the gold was due to HCN formed by decomposition of the explosive powder at high temperatures. Other associated reactions were also observed including the subsequent attack of the solder by the gold corrosion product and degradation of the plastic header.

Military aircraft use a cartridge ignition system for emergency engine starts. Analysis of premature failures of steel (AISI 4340) breech chambers in which the solid propellant cartridges were burned identified corrosion as one problem with an indication that stress-corrosion cracking may have occurred. A study was made for stress-corrosion cracking susceptibility of 4340 steel in a paste made of the residues collected from used breech chambers. The constant extension rate test (CERT) technique was employed and SCC susceptibility was demonstrated. The residues, which contained both combustion products from the cartridges and corrosion products from the chamber, were analyzed using elemental analysis and x-ray diffraction techniques. Electrochemical polarization techniques were also utilized to estimate corrosion rates.

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.

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.

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.

Following a freight train derailment, part of a fractured side frame was retained for study because a portion of its fracture surface exhibited a rock candy appearance and black scale. It was suspected of having failed, thereby precipitating the derailment. Metallography, scanning electron microscopy, EDXA, and x-ray mapping were used to study the steel in the vicinity of this part of the fracture surface. It was found to be contaminated with copper. Debye-Scherrer x-ray diffraction patterns obtained from the scale showed that it consisted of magnetite and hematite. It was concluded that some copper was accidentally left in the mold when the casting was poured. Liquid copper, carrying with it oxygen in solution, penetrated the austenite grain boundaries as the steel cooled. The oxygen reacted with the steel producing a network of scale outlining the austenite grain structure. When the casting fractured as a result of the derailment, the fracture followed the scale in the contaminated region thus creating the “rock candy” fracture.

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.

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.

In 1975, a manufacturer was awarded a contract to produce modular air-traffic control towers for the U.S. Navy. The specifications called for painted steel siding, but the manufacturer convinced the Navy to substitute aluminum-bonded-to-plywood panels that were provided by a supplier. In less than one year, the panels began to delaminate and the aluminum began to crack. It was found that the failure was the result of chloride-induced intergranular corrosion caused by chemicals in the adhesive and excessive moisture in the wood introduced during manufacturing.

Nickel anodes failed in several electrolysis cells in a heavy-water upgrading plant. Dismantling of a cell revealed gouging and the presence of loosely attached black porous masses on the anode. The carbon steel top, plate was severely corroded. An appreciable quantity of black powder was also present on the bottom or the cell. SEM/EDX studies of the outer and inner surfaces of the gouged anode showed the presence of iron globules at the interface between the gouged and the unattacked anode. The chemical composition of the black powder was determined to be primarily iron. Cell malfunction was attributed to the accelerated dissolution of the carbon steel anode top, dislodgment of grains from the material, and subsequent closing of the small annular space between the anode and the cathode by debris from the anode top. Cladding of the carbon steel top with a corrosion-resistant material, such as nickel, nickel-base alloy, or stainless steel, was recommended.

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.

Waterwall tube failure samples removed from a coal- and oil-fired boiler in service for 12 years exhibited localized underdeposit corrosion and hydrogen damage. EDS and XRD revealed that bulk internal deposits collected from the tubes contained metallic copper which can accelerate corrosion through galvanic effects and can promote hydrogen damage. Ultrasonic testing was recommended to locate tubes with severe gouging and corrosion, which are suspect locations for hydrogen damage. The source of the copper should be identified and future chemical cleaning of the boiler should address its presence in the waterwall tubes.

An investigation of the impeller and deposit samples from a centrifugal compressor revealed that an aluminum IR-12 refrigerant reaction had occurred, causing extensive damage to the second-stage impeller and contaminating the internal compressor components. The spherical surface morphology of the impeller fragments suggested that the aluminum had melted and resolidified. The deposits were similar in composition and were identified by XRD as consisting primarily of aluminum trifluoride. In addition, EDS analysis detected major amounts of chlorine and iron. Results of a combustion test indicated that the compressor deposit was comprised of a 9. 8 wt% carbon and that the condenser deposit contained 8.7 wt% carbon. It was concluded that the primary cause of failure was the rubbing of the impeller against the casting and that a self-sustaining Freon fire had occurred in the failed compressor

An arsenical admiralty brass (UNS C44300) finned tube in a generator air cooler unit at a hydroelectric power station failed. The unit had been in operation for approximately 49,000 h. Stereomicroscopic examination revealed two small transverse cracks that were within a few millimeters of the tube end, with one being a through-wall crack. Metallographic examination of sections containing the cracks showed branching secondary cracks and a transgranular cracking mode. The cracks appeared to initiate in pits. EDS analysis of a friable deposit found on the inside diameter of the tube and XRD analysis of crystalline compounds in the deposit indicated the possible presence of ammonia. Failure was attributed to stress-corrosion cracking resulting from ammonia in the cooling water. It was recommended that an alternate tube material, such as a 70Cu-30Ni alloy or a titanium alloy, be used.

Stress-corrosion cracking of low-alloy steel turbine discs has emerged as a generic concern in nuclear generating stations. An investigation that made extensive use of field metallographic techniques to examine suspected cracking in such a component is described. The crack position, and its relationship to surface topographic features, were examined and recorded by magnetic rubber and high-resolution dental rubber replicating materials. Corrosion deposits on keyway surfaces and within the crack were collected with acetate foil replicas applied and then stripped from the keyway surfaces. Microstructural details were revealed by the use of field metallographic preparation techniques and replicated by acetate foil for examination with optical and scanning electron microscopes. It was possible by these techniques to establish the cracking mechanism as stress corrosion possibly related to chloride or sulphate ion steam contaminants. Subsequent sectioning and conventional metallography confirmed both the validity of the conclusions and the replication techniques.