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.

An air blower in an electric power plant failed unexpectedly when a roller bearing in the drive motor fractured along its outer ring. Both rings, as well as the 18 rolling elements, were made from GCr15 bearing steel. The bearing also included a machined brass (MA/C3) cage and was packed with molybdenum disulfide (MoS 2 ) lithium grease. Metallurgical structures and chemical compositions of the bearing’s matrix materials were inspected using a microscope and photoelectric direct reading spectrometer. SEM/EDS was used to examine the local morphology and composition of fracture and contact surfaces. Chemical and thermal properties of the bearing grease were also examined. The investigation revealed that the failure was caused by wear due to dry friction and impact, both of which worsened as a result of high-temperature degradation of the bearing grease. Fatigue cracks initiated in the corners of the outer ring and grew large enough for a fracture to occur.

A 25 mm (1 in.) diam carrier shaft failed suddenly during operation. The shaft failed near the toe of the 4.8 mm (316 in.) frame-to-shaft 60 deg and 120 deg submerged metal arc (SMA) tack welds after an unknown time in service. Material specifications called for the shaft to be made from SAE 1018 cold-rolled carbon steel. Carrier assembly components were made from type 300 stainless steel, and all nuts, spacers, and washers were to be SMA tack welded to the stainless steel frame. Chemical analyses (OES, SEM/EDS) showed the shaft to actually be made from SAE 1050 high-carbon steel and that a low-carbon steel welding procedure had been used. This resulted in incipient cracks in the stainless steel weld metal near the toes of the component-to-shaft welds. The hardnesses of the heat-affected zones were as high as 58 HRC, and they were grain coarsened. The parting of the shaft was determined to have been caused by an impact failure mechanism, with the origin at the incipient cracks in the weld metal. Additionally, the coarsened heat-affected zones were found to be hydrogen embrittled. The primary cause of the failure was the use of an unspecified material.

A type 304 austenitic stainless steel tube (0.008 max C, 18.00 to 20.00 Cr, 2.00 max Mn, 8.00 to 10.50 Ni) was found to be corroded. The tube was part of a piping system, not yet placed in service, that was exposed to an outdoor marine environment containing chlorides. As part of the assembly, a fabric bag containing palladium oxide was taped to the tube. The palladium served as a “getter.” Investigation (visual inspection and EDS analysis of corrosion debris) supported the conclusion that chlorides and palladium both contributed to corrosion in the crevice created by the tape on the tube, which was periodically exposed to water. Recommendations included taking steps to prevent water from entering and being trapped in this area of the assembly.

A steel pot used as crucible in a magnesium alloy foundry developed a leak that resulted in a fire and caused extensive damage. Hypotheses as to the cause of the leak included a defect in the pot, overuse, overheating, and poor foundry practices. Scanning electron microscopy, transmission electron microscopy, optical microscopy, and x-ray microanalysis in conjunction with dimensional analysis, phase diagrams and thermodynamics considerations were employed to evaluate the various hypotheses. All evidence pointed to an oxide mass in the area where the hole developed, likely introduced during the steelmaking process.

Microstructural examinations on transverse cross sections of a steam reformer tube, showed the presence of large macrovoids elongated in the radial direction and emanating from the internal surface of the tube. The macrovoids were located at the interdendritic regions, and were partially filled by a Mn-Fe bearing chromium oxide film. The areas adjacent to the oxide film were chemically depleted in C, Cr and Mn and rich in Fe and Ni. Associated with this depletion were a large concentration of microvoids. It was suggested that the dissolution of carbides in areas surrounding the macrovoids and the concentration of stresses at their tips, caused extensive localized plastic deformation which led to the formation of microvoids and subsequently to the spalling of the oxide film. The non-protective character of the film induced a progressive deterioration of the grain boundaries properties. Grain boundary sliding and dislocation motion were enhanced, causing a local increase in the steady state strain rate and the premature failure of the tube.

The crosslinked epoxy resin encapsulant protecting an electromagnetic valve coil failed during long-term storage and was examined to determine the cause. The investigation included fault-tree analysis, FTIR and EDX spectroscopy, and differential scanning calorimetry with thermogravimetric analysis. Based on test data, the epoxy resin had not been properly cured and was hydrolyzed in its compromised state because of humidity. Hence, the depolymerized material gradually softened to the point where the effect of creep caused it to flow, ultimately causing the failure.

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.

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.

Two clamps that support overhead power lines in an electrified rail system fractured within six months of being installed. The clamps are made of CuNiSi alloy, a type of precipitation-strengthening nickel-silicon bronze. To identify the root cause of failure, the rail operator led an investigation that included fractographic and microstructural analysis, hardness testing, inductively coupled plasma spectroscopy, and finite-element analysis. The fracture was shown to be brittle in nature and covered with oxide flakes, but no other flaws relevant to the failure were observed. The investigation results suggest that the root cause of failure was a forging lap that occurred during manufacturing. Precracks induced by the forging defect and the influence of preload stress (due to bolt torque) caused the premature failure.

The case study presented in this article details the failure investigation of an M50 alloy steel bearing used in a jet engine gearbox drive assembly. It discusses the investigative steps and analytic tools used to determine the root cause, highlighting the importance of continuous, thorough questioning by the investigating activity. The combined analyses demonstrated that the bearing failed by a single event overload as evidenced by bulk deformation and traces of foreign material on the rolling elements. The anomalous transferred metal found on the rolling elements subsequently led to the discovery of overlooked debris in an engine chip detector, and thus resulted in a review of several maintenance practices.

This paper summarizes several cases of metallurgical failure analysis of surgical implants conducted at the Laboratory of Failure Analysis of IPT, in Brazil. Investigation revealed that most of the samples were not in accordance with ISO standards and presented evidence of corrosion assisted fracture. Additionally, some components were found to contain fabrication/processing defects that contributed to premature failure. The implant of nonbiocompatible materials results in immeasurable damage to patients as well as losses for the public investment. It is proposed that local sanitary regulation agencies create mechanisms to avoid commercialization of surgical implants that are not in accordance with standards and adopt the practice of retrieval analysis of failed implants. This would protect the public health by identifying and preventing the main causes of failure in surgical implants.

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.

A heavy duty facing lathe failed when the tool post caught one of the jaws on the rotating chuck, causing the spline shaft that drives the main spindle to fracture. A detailed analysis of the fracture surfaces (including fractography, metallography, and analytical stress calculations) revealed areas of damage due to rubbing with evidence of cleavage fracture on the unaffected surfaces. The results of stress analysis indicated that repeated reversals of the spindle produced stresses exceeding the fatigue limit of the shaft material. These stresses led to the formation of microcracks in a retaining ring groove that were accelerated to sudden failure when the tool post and chuck collided.

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 commercial hybrid-iron golf club fractured during normal use. The club fractured through its cast aluminum alloy hosel. Optical analysis revealed casting pores through 20% of the hosel thickness. Mechanical properties were determined from characterization results, then used to construct a finite element model to analyze material performance under failure conditions. In addition, a full scale structural test was conducted to determine failure strength. It was concluded that the club failed not from ground impact but from a force reversal at the bottom of the downswing. Large moments generated during the downswing aggravated by manufacturing defects and stress concentration combined to create an overload condition.

The interior surface of a type 316L stainless steel trailer barrel used to haul various chemicals showed evidence of severe pitting after less than 1 year of service. Two sections were cut from the barrel and microscopically examined. Metallographic sections were also prepared at the weld areas and away from the weld zones. Terraced, near-surface pits with subsurface caverns and a high level of sulfur in the pit residue, both indicative of bacteria-induced corrosion, were found. No evidence of weld defects or defective material was present. Testing of the water used at the wash station and implementation of bacteria control measures (a special drying process after washing and use of a sanitizing rinse) were recommended.

Recurring, premature failures occurred in TiN-coated M2 gear hobs used to produce carbon steel ring gears. Fractographic and metallographic examination, microhardness testing, and chemical analysis by means of EDS revealed that the primary cause of failure was a coarse cellular carbide network, which created a brittle path for fracture to occur longitudinally. As the cellular carbide network must be dispersed and refined during hot working of the original bar of material, the hobs were not salvageable. Minor factors contributing to the hob failures were premature wear resulting from lower matrix hardness and high sulfur content of the material, which contributed to lower ductility through increased nucleation sites. It was recommended that the hob manufacturer specify a minimum amount of required reduction for the original bar of tool steel material, to provide for sufficient homogenization of the carbides in the resultant hob, and lower sulfur content.

Failure analysis of a mobile harbor crane wheel hub that included SEM and EDS analyses demonstrated that the mechanism of failure was fatigue. The wheel hub was a ductile cast iron component that had been subjected to cyclic loading during a ten-year service period. The fracture surface of the fatigue failure also contained corrosion deposit, suggesting that cracking occurred over a period of time sufficient to allow corrosion of the cracked surfaces. Replacement and alignment of the failed wheel hub was recommended along with inspection of the nonfailed wheel hubs that remained on the crane.