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.

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.

This article provides practical information and data on property development in engineering plastics. It discusses the effects of composition on submolecular and higher-order structure and the influence of plasticizers, additives, and blowing agents. It examines stress-strain curves corresponding to soft-and-weak, soft-and-tough, hard-and-brittle, and hard-and-tough plastics and temperature-modulus plots representative of polymers with different degrees of crystallinity, cross-linking, and polarity. It explains how viscosity varies with shear rate in polymer melts and how processes align with various regions of the viscosity curve. It discusses the concept of shear sensitivity, the nature of viscoelastic properties, and the electrical, chemical, and optical properties of different plastics. It also reviews plastic processing operations, including extrusion, injection molding, and thermoforming, and addresses related considerations such as melt viscosity and melt strength, crystallization, orientation, die swell, melt fracture, shrinkage, molded-in stress, and polymer degradation.

Identification of alloys using quantitative chemical analysis is an essential step during a metallurgical failure analysis process. There are several methods available for quantitative analysis of metal alloys, and the analyst should carefully approach selection of the method used. The choice of appropriate analytical techniques is determined by the specific chemical information required, the condition of the sample, and any limitations imposed by interested parties. This article discusses some of the commonly used quantitative chemical analysis techniques for metals. The discussion covers the operating principles, applications, advantages, and disadvantages of optical emission spectroscopy (OES), inductively coupled plasma optical emission spectroscopy (ICP-OES), X-ray spectroscopy, and ion chromatography (IC). In addition, information on combustion analysis and inert gas fusion analysis is provided.

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.

This article describes the processes involved in photochemical aging and weathering of polymeric materials. It explains how solar radiation, especially in the UV range, combines with atmospheric oxygen, driving photooxidation and the development of unstable photoproducts that cause various types of damage when they decompose, including the scission of carbon bonds and polymer chains. The article illustrates some of the degradation reactions that occur in different polymers and presents an overview of the strategies used to prevent such reactions or otherwise mitigate their effects.

The rear wall tube section of a boiler that had been in service for approximately 38 years was removed and examined. Visual examination of the tube revealed a small bulge with a through-wall crack. Metallography showed that the microstructure of the bulged area consisted of a few partially decarburized pearlite colonies in a ferrite matrix. The microstructure remote from the bulged area consisted of pearlite in a ferrite matrix. EDS analysis of internal deposits on the tube detected a major amount of iron, plus trace amounts of other elements. The evidence indicated that the bulge and crack in the tube resulted from hydrogen damage. Examination of the remaining water circuit boiler tubing using nondestructive techniques and elimination of any heavy deposit buildup was recommended.

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.

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.

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 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.

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.

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.

The article commences with an overview of short-term and long-term mechanical properties of polymeric materials. It discusses plasticization, solvation, and swelling in rubber products. The article further describes environmental stress cracking and degradation of polymers. It illustrates how surface degradation of a plain strain tension specimen alters the ductile brittle transition in polyethylene creep rupture. The article concludes with information on the effects of temperature on polymer performance.

This article provides an overview of the classification of hydrogen damage. Some specific types of the damage are hydrogen embrittlement, hydrogen-induced blistering, cracking from precipitation of internal hydrogen, hydrogen attack, and cracking from hydride formation. The article focuses on the types of hydrogen embrittlement that occur in all the major commercial metal and alloy systems, including stainless steels, nickel-base alloys, aluminum and aluminum alloys, titanium and titanium alloys, copper and copper alloys, and transition and refractory metals. The specific types of hydrogen embrittlement discussed include internal reversible hydrogen embrittlement, hydrogen environment embrittlement, and hydrogen reaction embrittlement. The article describes preservice and early-service fractures of commodity-grade steel components suspected of hydrogen embrittlement. Some prevention strategies for design and manufacturing problem-induced hydrogen embrittlement are also reviewed.

Hydrogen damage is a term used to designate a number of processes in metals by which the load-carrying capacity of the metal is reduced due to the presence of hydrogen. This article introduces the general forms of hydrogen damage and provides an overview of the different types of hydrogen damage in all the major commercial alloy systems. It covers the broader topic of hydrogen damage, which can be quite complex and technical in nature. The article focuses on failure analysis where hydrogen embrittlement of a steel component is suspected. It provides practical advice for the failure analysis practitioner or for someone who is contemplating procurement of a cost-effective failure analysis of commodity-grade components suspected of hydrogen embrittlement. Some prevention strategies for design and manufacturing problem-induced hydrogen embrittlement are also provided.

High temperature corrosion may occur in numerous environments and is affected by factors such as temperature, alloy or protective coating composition, time, and gas composition. This article explains a number of potential degradation processes, namely, oxidation, carburization and metal dusting, sulfidation, hot corrosion, chloridation, hydrogen interactions, molten metals, molten salts, and aging reactions including sensitization, stress-corrosion cracking, and corrosion fatigue. It concludes with a discussion on various protective coatings, such as aluminide coatings, overlay coatings, thermal barrier coatings, and ceramic coatings.

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

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.

With any polymeric material, chemical exposure may have one or more different effects. Some chemicals act as plasticizers, changing the polymer from one that is hard, stiff, and brittle to one which is softer, more flexible, and sometimes tougher. Often these chemicals can dissolve the polymer if they are present in large enough quantity and if the polymer is not crosslinked. Other chemicals can induce environmental stress cracking (ESC), an effect in which brittle fracture of a polymer will occur at a level of stress well below that required to cause failure in the absence of the ESC reagent. Finally, there are some chemicals that cause actual degradation of the polymer, breaking the macromolecular chains, reducing molecular weight, and diminishing polymer properties as a result. This article examines each of these effects. The discussion also covers the effects of surface embrittlement and temperature on polymer performance.