A batch of bimetal foil/epoxy laminates was rejected because of poor peel strength. The laminates were manufactured by sintering a nickel/phosphorus powder layer to a copper foil, cleaning, then chromate conversion coating the nickel-phosphorus surface, and laminating the nickel-phosphorus side of the clad bimetal onto an epoxy film, so that the end product contained nickel-phosphorus sandwiched between copper and epoxy, with a chromate conversion layer on the epoxy side of the nickel-phosphorus. Peel testing showed abnormally low adhesion strength for the bad batch of peel test samples. Comparison with normal-strength samples using XPS indicated an 8.8% Na concentration on the surface of the bad sample; the good example contained less than 1% Na on the surface. After 15 min of argon ion etching, depth profiling showed high concentrations of sodium were still evident, indicating that the sodium was present before the chromate conversion treatment was performed. A review of the manufacturing procedures showed that sodium hydroxide was used as a cleaning agent before the chromate conversion coating. Failure cause was that apparently the sodium hydroxide had not been properly removed during water rinsing. Thus, recommendation was to modify that stage in the processing.

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 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.

The failure of a boiler operating at 540 °C and 9.4 MPa was investigated by examining material samples from the near-failure region and by thermodynamic analysis. A scanning Auger microprobe, SEM, and commercial thermodynamic software codes were used in the investigation. Results indicated that the boiler failure was caused by grain-boundary segregation of phosphorous, tin, and nitrogen and the in-service formation of carbide films and granules on the grain boundaries.

The causes of internal cracking that occurred in 9% Ni steel castings during manufacture were investigated using a series of eight laboratory castings containing varying amounts of molybdenum. The effect of mold thickness was also investigated. The laboratory castings were subjected to three-point bend testing, and fracture surfaces were examined using SEM fractography, metallography, and depth analysis (SIMS) of the fracture surface. The cracks were found to originate at austenitic grain boundaries that coincided with primary dendrite interfaces. The cracking was attributed to a decrease in grain-boundary cohesion resulting from sulfur segregation. Addition of molybdenum proved effective in preventing cracking. The molybdenum promoted MnS precipitation in the grain and preferentially segregated to the interfaces.

A steel spring used in an automotive application suddenly began to fail in the field, although “nothing had changed” in the fabrication process. Fatigue tests using springs fabricated prior to field failures lasted 500,000 cycles to failure, whereas fatigue tests performed on springs fabricated after field failures lasted only 50,000 cycles to failure. It was discovered that the percent coverage of shot peening prior and subsequent to the increase in failure incidence was much less than 100%, with a shot peening time of 12 min. The residual-stress state of “as fabricated” springs in three conditions were evaluated using XRD: springs manufactured prior to failure incidence increase, 12 min peen; springs manufactured following failure incidence increase, 12 min peen; and 60 min peen. The conclusion was that the failure occurred because low peening time significantly decreased the compressive residual-stress levels in the springs. Recommendation was made to increase the time the spring was shot peened from 12 to 60 min.

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.

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.

An investigation of a damaged crankshaft from a horizontal, six-cylinder, in-line diesel engine of a public bus was conducted after several failure cases were reported by the bus company. All crankshafts were made from forged and nitrided steel. Each crankshaft was sent for grinding, after a life of approximately 300,000 km of service, as requested by the engine manufacturer. After grinding and assembling in the engine, some crankshafts lasted barely 15,000 km before serious fractures took place. Few other crankshafts demonstrated higher lives. Several vital components were damaged as a result of crankshaft failures. It was then decided to send the crankshafts for laboratory investigation to determine the cause of failure. The depth of the nitrided layer near fracture locations in the crankshaft, particularly at the fillet region where cracks were initiated, was determined by scanning electron microscope (SEM) equipped with electron-dispersive X-ray analysis (EDAX). Microhardness gradient through the nitrided layer close to fracture, surface hardness, and macrohardness at the journals were all measured. Fractographic analysis indicated that fatigue was the dominant mechanism of failure of the crankshaft. The partial absence of the nitrided layer in the fillet region, due to over-grinding, caused a decrease in the fatigue strength which, in turn, led to crack initiation and propagation, and eventually premature fracture. Signs of crankshaft misalignment during installation were also suspected as a possible cause of failure. In order to prevent fillet fatigue failure, final grinding should be done carefully and the grinding amount must be controlled to avoid substantial removal of the nitrided layer. Crankshaft alignment during assembly and proper bearing selection should be done carefully.

A ‘worn-out’ spiral bevel gear and pinion set was submitted for examination and evaluation. This was a spiral bevel drive set with the gear attached to a differential. The assembled unit was driving a new, large, experimental farm tractor in normal plowing and tilling operations. The primary failure was associated with the 4820H NiMo alloy steel pinion, and thus the gear was not examined. The mode of failure was rolling contact fatigue, and the cause of failure improper engineering design. The pattern of continual overload was restricted to a specific concentrated area situated diagonally across the profile of the loaded side, which was consistent on every tooth.

An investigation was conducted to determine what caused a bearing sleeve in a locomotive turbocharger to fail. The sleeve, which is made of nitrided 38CrMoAl steel, fractured at the transition fillet between the cylinder and plate. Visual examination revealed significant wear on the external surface of the cylinder, with multiple origin fatigue fracture appearing to be the dominant fracture mechanism. Metallurgical examination indicated that the nitrided layer was not as deep as it was supposed to be and had worn away on the outer surface of the sleeve, exposing the soft matrix underneath. This led to further wear and an increase in friction between the sleeve and bearing bush. Fatigue crack initiation occurred at the root fillet because of stress concentration and large frictional forces. Insufficient nitriding depth facilitated the propagation of fatigue cracks.

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.

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 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.

During construction of a river bridge with 80 twisted cables, one or more fractures were found in each of 21 wires of 18 cables before assembly. All were located at the outside wrapping whose Z-profile wires were galvanically zinc-coated. It was suspected that hydrogen played a role during crack formation, and that it penetrated during pickling or galvanizing. This supposition was confirmed also by the fact that the wire fractures were not observed during cable winding, but only subsequently to it, and therefore seemed to have appeared only after a certain delay.