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 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.

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.

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 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.

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.

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.

Within the first few months of operation of an 8 km (5 mile) long 455 mm (18 in.) diam high-pressure steam line between a coal-fired electricity-generating plant and a paper mill, several of the Inconel 600 bellows failed. The steam line operated at 6030 kPa (875 psi) and 420 deg C (790 deg F). Metallographic sections, energy-dispersive x-ray spectra, chemical analyses, tensile tests, and Auger microscope analyses showed the failed bellows met the specifications for the material. However, investigation also showed entire oxide thickness was contaminated with relatively large amounts of sodium, calcium, potassium, aluminum, and sulfur, alkali, alkali earth, and other contaminants that completely permeated even the thin oxides on the fracture surfaces. Additional investigation of the purity of the steam itself as reported by the power plant showed that corrosion and cracks were ultimately caused by the steam. While under normal operation, the steam's purity posed no problem to the material, during boiler cleaning operations, the generating plant had allowed contamination to get into the steam line.

A failure analysis case study on railroad rails is presented. The work, performed under the sponsorship of the Department of Transportation, addresses the problem of shell and detail fracture formation in standard rails. Fractographic and metallographic results coupled with hardness and residual stress measurements are presented. These results suggest that the shell fractures form on the plane of maximum residual tensile stresses. The formation of the shells is aided by the presence of defects in the material in these planes of maximum residual stress. The detail fracture forms as a perturbation from the shell crack under cyclic loading and is constrained to develop as an embedded flaw in the early stages of growth because the crack is impeded at the gage side and surface of the rail head by compressive longitudinal stresses.

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.

The US Army Research Laboratory performed a failure investigation on a broken main landing gear mount from an AH-64 Apache attack helicopter. A component had failed in flight, and initially prevented the helicopter from safely landing. In order to avoid a catastrophe, the pilot had to perform a low hover maneuver to the maintenance facility, where ground crews assembled concrete blocks at the appropriate height to allow the aircraft to safely touch down. The failed part was fabricated from maraging 300 grade steel (2,068 MPa [300 ksi] ultimate tensile strength), and was subjected to visual inspection/light optical microscopy, metallography, electron microscopy, energy dispersive spectroscopy, chemical analysis, and mechanical testing. It was observed that the vacuum cadmium coating adjacent to the fracture plane had worn off and corroded in service, thus allowing pitting corrosion to occur. The failure was hydrogen-assisted and was attributed to stress corrosion cracking (SCC) and/or corrosion fatigue (CF). Contributing to the failure was the fact that the material grain size was approximately double the required size, most likely caused from higher than nominal temperatures during thermal treatment. These large grains offered less resistance to fatigue and SCC. In addition, evidence of titanium-carbo-nitrides was detected at the grain boundaries of this material that was prohibited according to the governing specification. This phase is formed at higher thermal treatment temperatures (consistent with the large grains) and tends to embrittle the alloy. It is possible that this phase may have contributed to the intergranular attack. Recommendations were offered with respect to the use of a dry film lubricant over the cadmium coated region, and the possibility of choosing an alternative material with a lower notch sensitivity. In addition, the temperature at which this alloy is treated must be monitored to prevent coarse grain growth. As a result of this investigation and in an effort to eliminate future failures, ARL assisted in developing a cadmium brush plating procedure, and qualified two Army maintenance facilities for field repair of these components.

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.

A forged aluminum alloy 2014-T6 catapult-hook attachment fitting (anodized by the chromic acid process to protect it from corrosion) from a naval aircraft broke in service. Spectrographic analysis, visual examination, microscopic examination, and tensile analysis showed minute cracks on the inside surface of a bearing hole, and small areas of pitting corrosion were visible on the exterior surface of the fitting. The analysis also revealed a small number of rosettes, suggestive of eutectic melting, in an otherwise normal structure. These examinations and analyses support the conclusion that the presence of chromic acid stain on the fracture surface proved that the forging had cracked before anodizing. This suggest that the crack initiated during straightening, either after machining or after heat treatment. The structure and composition of the alloy appear to have been acceptable. Ductility was acceptable so rosettes found in the microstructure are believed to have been nondamaging. Had they contributed to the failure, the ductility would have been very low. The recommendations included inspection for cracks and revising the manufacturing process to include a fluorescent liquid-penetrant inspection before anodizing, because chromic acid destroys the penetrant. This inspection would reduce the possibility of cracked parts being used in service.

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.

A nuclear steam-generator vessel constructed of 100-mm thick SA302, grade B, steel was found to have a small leak. The leak originated in the circumferential closure weld joining the transition cone to the upper shell. The welds had been fabricated from the outside by the submerged arc process with a backing strip. The backing was back gouged off, and the weld was completed from the inside with E8018-C3 electrodes by the shielded metal arc process. Striations of the type normally associated with progressive or fatigue-type failures including beach marks that allowed tracing the origin of the fracture to the pits on the inner surface of the vessel were revealed. Copper deposits with zinc were revealed by EDS examination of discolorations. Pitting was revealed to have been caused by poor oxygen control in the steam generators and release of chloride into the steam generators. It was concluded by series of controlled crack-propagation-rate stress-corrosion tests that A302, grade B, steel was susceptible to transgranular stress-corrosion attack in constant extension rate testing with as low as 1 ppm chloride present. It was recommended to maintain the coolant environment low in oxygen and chloride. Copper ions in solution should be eliminated or minimized.

Pendant-style reheater, constructed of ASME SA-213, grade T-11, steel ruptured. A set of four tubes, specified to be 64 mm OD x 3.4 mm minimum wall thickness was examined. A small quantity of loose debris was removed from the inside of one of the tubes. The major constituent was revealed by EDS analysis of the debris to be iron with traces of phosphorus, manganese, sodium, calcium, copper, zinc, potassium, silicon, chromium, and molybdenum. Thus the debris was interpreted to be the scale from ID of the tube with boiler feedwater chemicals from the attemperation spray. The likely cause of failure was concluded to be exfoliation of the scale from the ID surface of the tube. Creep failures were interpreted to be caused by localized temperatures higher than the maximum service temperature. Replacement of the affected tubes was recommended. Inspection of the tubes by radiography to find the circuits with the greatest accumulation of debris and replacing them as necessary was recommended on an annual basis.

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. The cooling medium for the tubes was water from a river. Air flowed over the finned exterior of the tubes, while water circulated through the tubes. Investigation (visual inspection, leak testing, history review, 100X micrographs etched in potassium dichromate, chemical analysis, and EDS and XRD analysis of internal tube deposits) supported the conclusion that the cause of the tube leaks was ammonia-induced SCC. Because the cracks initiated on the inside surfaces of the tubes and because the river water was not treated before it entered the coolers, the ammonia was likely present in the river water and probably concentrated under the internal deposits. Recommendations included either eliminating the ammonia (prohibitively expensive in cost and time) or using an alternate material (such as a 70Cu-30Ni alloy or a more expensive titanium alloy) that is resistant to ammonia corrosion as well as to chlorides and sulfur species.

A brazing-furnace muffle 34 cm (13 in.) wide, 26 cm (10 in.) high, and 198 cm (78 in.) long, was fabricated from nickel-base high-temperature alloy sheet and installed in a gas-fired furnace used for copper brazing of various assemblies. The operating temperature of the muffle was reported to have been closely controlled at the normal temperature of 1175 deg C (2150 deg F); a hydrogen atmosphere was used during brazing. After about five months of continuous operation, four or five holes developed on the floor of the muffle, and the muffle was removed from service. Analysis (visual inspection, x-ray spectrometry, and metallographic examination) supported the conclusion that the muffle failed by localized overheating in some areas to temperatures exceeding 1260 deg C (2300 deg F). The copper found near the holes had dripped to the floor from assemblies during brazing. The copper diffused into the nickel-base alloy and formed a grain-boundary phase that was molten at the operating temperature. The presence of this phase caused localized liquefaction and weakened the alloy sufficiently to allow formation of the holes. No recommendations were made.

One of 14 vertical radiant tubes (RA 333 alloy) in a heat-treating furnace failed when a hole about 5 x 12.5 cm (2 x 5 in.) corroded completely through the tube wall. The tube measured 183 cm (72 in.) in length and 8.9 cm (3 in.) in OD and had a wall thickness of about 3 mm (0.120 in.). Failure occurred where the tube passed through the refractory hearth (floor) of the furnace. Although the furnace atmosphere was neutral with respect to the work, it had a carburizing potential relative to the radiant tubes. Analysis (visual inspection, 250x spectroscopic examination of specimens etched with mixed acids, metallographic examination, and chemical analysis) supported the conclusions that the premature failure of the tube by perforation at the hearth level resulted from (1) corrosion caused by sulfur contamination from the refractory cement in contact with the tube and (2) severe local overheating at the same location. Recommendations included replacing all tubes using a low sulfur refractory cement in installation and controlling burner positioning and regulation more closely to avoid excessive heat input at the hearth level.

A kiln, 7.6 m (25 ft) long with a 1 m (3 ft) internal diameter and a 6.3 mm (0.25 in.) wall thickness, is used to regenerate spent charcoal returned by water utilities. This charcoal contains up to 0.57% S and 2.04% Cl. The kiln is made of Inconel 601 (N06601) welded using Inconel 617 (N06617) as a filler alloy. Wet charcoal is fed in at one end of the kiln and travels while being tumbled within the inclined rotating vessel. Temperatures range from 480 deg C (900 deg F) (Zone 1) to 900 deg C (1650 deg F) (Zones 2 and 3). Steam is introduced at the discharge end at 95 g/s (750 lb/h), 34 to 69 kPa (5 to 10 psi), and 125 deg C (260 deg F). The kiln developed perforations within eight months of operation. Investigation (visual inspection, metallurgical analysis, energy-dispersive spectroscopy, and 44X micrographs) supported the conclusion that the sulfur and chlorine in the charcoal attacked the Inconel 601, forming various sulfides and chlorides. Recommendations included on-site testing, and installation of test coupons of various alloys before fabricating another kiln. The suggested alloys were RA85H, 800HT, HR-120, Haynes 556, and HR-160.