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.

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.

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.

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.

A nickel alloy cylinder plated with chromium along its inner liner, installed in a commercial ice cream freezer, showed gray discoloration along its OD surface. The discolored parts exhibited significantly reduced cooling efficiency as compared with new cylinders. During operation, the OD of the cylinder was exposed to liquid ammonia refrigerant containing lubricant from the compressor. The lubricant (mineral oil) was intended to separate from the ammonia and be recirculated through the compressor. Nondestructive portable optical microscopy, XRF, EDS, and XPS analyses showed that the discoloration on the cylinder was associated with metal oxidation products coated with a thin oil film. One of the recommendations was to plate the OD of the cylinder with hard chromium to increase its resistance to erosion. Another recommendation was to reduce the amounts of water contamination in the refrigerant.

The rear outside wheel of an over-the-road 18-wheel tractor-trailer failed at its bolt holes, permitting the tire and wheel to separate from the hub. Failure analysis was conducted using photographic examination of actual fracture surfaces and SEM examination of fracture replicas. The examinations indicated that fatigue cracks had originated at the rim backside and propagated to the rim midsection. Catastrophic failure occurred at a final overland. Fatigue fracture of the wheel rim was attributed to cyclic loading created by improper wheel mounting of a spare tire.

A large number of electropolished copper parts showed evidence of discoloration (tinting) after electropolishing. Because these parts are used in a high-vacuum application, even trace amounts of organic materials would be problematic. Scanning electron microscopy of nondiscolored and discolored areas both showed trace amounts of residue in the form of adherent deposits. EDS, FTIR spectroscopy, XPS, and secondary ion mass spectroscopy (SIMS) analyses indicated that the discoloration to the copper components was due to the development of CuO at localized regions. It was recommended that process changes be made to completely remove residual processing fluids from the part surfaces before electropolishing. The use of more aggressive detergents was suggested, and it was recommended also that a filtering and recirculating system be considered for use in the cleaning and electropolishing tanks.

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.

This paper deals with disk drive failures that occur in the interface area between the head and disk. The failures often lead to the loss of stored data and are characterized by circumferential microscratches that are usually visible to the unaided eye. The recording media in disk drives consists of a metal, glass, ceramic, or plastic substrate coated with a magnetic material. Data errors are classified as ‘soft’ or ‘hard’ depending on their correctability. Examination has shown that hard errors are the result of an abrasive wear process that begins with contact between head and disk asperities. The contact generates debris that, as it accumulates, increases contact pressure between the read-write head and the surface of the disk. Under sufficient pressure, the magnetic coating material begins wearing away, resulting in data loss.

A major cause of failure in components subjected to rolling or rolling/sliding contacts is contact fatigue. This article focuses on the rolling contact fatigue (RCF) performance and failure modes of overlay coatings such as those deposited by physical vapor deposition, chemical vapor deposition, and thermal spraying (TS). It provides a background to RCF in bearing steels in order to develop an understanding of failure modes in overlay coatings. The article describes the underpinning failure mechanisms of TiN and diamond-like carbon coatings. It presents an insight into the design considerations of coating-substrate material properties, coating thickness, and coating processes to combat RCF failure in TS coatings.

Six transformer brackets failed in service, sending a group of three pole-mounted transformers to the ground below. The brackets were made from acrylonitrile-butadiene-styrene (ABS) resin and had been in service for more than 30 years. Remnants of the fractured brackets were analyzed using optical and scanning electron microscopy, Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). The exterior surfaces of all six brackets were alike and shared similar features, including witness marks, discoloration, mechanical deformation, and secondary cracking, along with crack networks. Both FTIR and TGA analyses indicated that the surface material was in a highly degraded state, likely due to weathering and thermal and ultraviolet exposure. This, in turn, led to the formation of cracks that propagated under the cyclic forces of vibration and wind. As the cracks grew larger, the weight of the transformer eventually overloaded the brackets, resulting in failure.

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 of three C22000 commercial bronze rupture discs was caused by mercury embrittlement. The discs were part of flammable gas cylinder safety devices designed to fail in a ductile mode when cylinders experience higher than design pressures. The subject discs failed prematurely below design pressure in a brittle manner. Fractographic examination using SEM indicated that failure occurred intergranularly from the cylinder side. EDS analysis indicated the presence of mercury on the fracture surface and mercury was also detected using scanning auger microprobe (SAM) analysis. The mercury was accidentally introduced into the cylinders during a gas-blending operation through a contaminated blending manifold. Replacement of the contaminated manifold was recommended along with discontinued use of mercury manometers, the original source of mercury contamination.

The scanning electron microscopy (SEM) is one of the most versatile instruments for investigating the microstructure of metallic materials. This article highlights the development of SEM technology and describes the operation of basic systems in an SEM, including the electron optical column, signal detection and display equipment, and vacuum system. It discusses the preparation of samples for observation using an SEM and describes the application of SEM in fractography. If the surface remains unaffected and undamaged by events subsequent to the actual failure, it is often a simple matter to determine the failure mode by the use of an SEM. In cases where the surface is altered after the initial failure, the case may not be so straightforward. The article presents typical examples that illustrate these points. Image dependence on the microscope type and operating parameters is also discussed.

This article commences with a summary of fatigue processes and mechanisms. It focuses on fractography of fatigue. Characteristic fatigue fracture features that can be discerned visually or under low magnification are described. Typical microscopic features observed on structural metals are presented subsequently, followed by a brief discussion of fatigue in nonmetals. The article reviews the various macroscopic and microscopic features to characterize the history and growth rate of fatigue in metals. It concludes with a description of fatigue of polymers and composites.

The scanning electron microscope (SEM) is one of the most versatile instruments for investigating the microscopic features of most solid materials. The SEM provides the user with an unparalleled ability to observe and quantify the surface of a sample. This article discusses the development of SEM technology and operating principles of basic systems of SEM. The basic systems covered include the electron optical column, signal detection and display equipment, and the vacuum system. The processes involved in the preparation of samples for observation using an SEM are described, and the application of SEM in fractography is discussed. The article covers the failure mechanisms of ductile failure, brittle failure, mixed-mode failure, and fatigue failure. Lastly, image dependence on microscope type and operating parameters is also discussed.