Search Results for SEM backscattered electron analysis

An investigation was conducted to determine why 16 out of 139 pipe bends cracked during hot induction bending. The pipe conformed to API 5L X65 PSL2 line pipe standards and measured 1016 mm (40 in.) in diam with a wall thickness of 18.5 mm. A metallurgical cross section was removed along a crack on the extrados to document the crack morphology using optical microscopy. In addition to cracking, golden-yellow streaks were visible at the extrados, and the composition was examined using scanning electron microscopy with energy dispersive spectroscopy. Based on the results, investigators concluded the pipe was contaminated with copper at the mill were it was produced.

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.

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.

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.

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.

Chemical analysis is a critical part of any failure investigation. With the right planning and proper analytical equipment, a myriad of information can be obtained from a sample. This article presents a high-level introduction to techniques often used for chemical analysis during failure analysis. It describes the general considerations for bulk and microscale chemical analysis in failure analysis, the most effective techniques to use for organic or inorganic materials, and examples of using these techniques. The article discusses the processes involved in the chemical analysis of nonmetallics. Advances in chemical analysis methods for failure analysis are also covered.

The failure of T12 reheater tubes that had been in service for only 3000 h was investigated. The thickness of the tubes was visibly reduced by heavy oxidation corrosion on the inner and outer walls. The original pearlite substrate completely decomposed. Uniform oxide scale observed on the inner wall showed obvious vapor oxidation corrosion characteristics. Corrosion originated in the grain boundary, and selective oxidation occurred due to ion diffusion in the substrate. The layered oxide scale on the inner wall is related to the different diffusion rates for different cations. Exposure to high temperature corrosive flux accelerated the corrosion on the outer wall. Microstructure degradation and the corrosion characteristics observed indicate that the tubes failed primarily because of overheating, which is confirmed by calculations.

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.

Admiralty brass (Alloy C44300) cooling tubes which were part of a heat exchanger in a turbogenerator that provided electricity to a manufacturing plant failed. A mixture of non-recirculating city and “spring pit” water flowed through bundles of tubes to cool the oil in which they are immersed. However, a problem developed when several of the brass tubes cracked transversely, allowing cooling water to mix with the oil. The presence of a tensile stress, intergranular cracks, and a corrosion product suggested the tube failures resulted from stress-corrosion cracking. The main corrosion product was cupric hydroxychloride. In addition to switching to a more corrosion-resistant alloy, extreme care should be taken in the manufacturing of the replacement tube bundles to avoid imparting any residual tensile stresses in the tubing. Analyses of city and spring-pit water were recommended also, to determine which contained the least-harmful corrosive chemicals.

Four cadmium-plated ASTM A193 grade B studs from a steam line connector associated with a power turbine failed unexpectedly in a nil-ductility manner. Fracture surfaces were covered with a light-colored, lustrous deposit. Optical microscope, SEM, and EDS analyses were conducted on sections from one of the studs and revealed that the coating on the fracture surface was cadmium. The fracture had multiple origins, and secondary cracks also contained cadmium. The fracture topography was intergranular. The failures were attributed to liquid metal embrittlement caused by the presence of a cadmium plating and operating temperatures at approximately the melting point of cadmium. It was recommended that components exposed to the cadmium be replaced.

This paper describes an investigation on the failure of a large leaded bronze bearing that supports a nine-ton roller of a plastic calendering machine. At the end of the normal service life of a good bearing, which lasted for seven years, a new bearing was installed. However the new one failed catastrophically within a few days, generating a huge amount of metallic wear debris and causing pitting on the surface of the cast iron roller. Following the failure, samples were collected from both good and failed bearings. The samples were analyzed chemically and their microstructures examined. Both samples were subjected to accelerated wear tests in a laboratory type pin-on-disk apparatus. During the tests, the bearing materials acted as pins, which were pressed against a rotating cast iron disk. The wear behaviors of both bearing materials were studied using weight loss measurement. The worn surfaces of samples and the wear debris were examined by light optical microscope, SEM, and energy-dispersive x-ray microanalyzer. It was found that the laboratory pin-on-disk wear data correlated well with the plant experience. It is suggested that the higher lead content ~18%) of the good bearing compared with 7% lead of the failed bearing helped to establish a protective transfer layer on the worn surface. This transfer layer reduced metal-to-metal contact between the bearing and the roller and resulted in a lower wear rate. The lower lead content of the failed bearing does not allow the establishment of a well-protected transfer layer and leads to rapid wear.

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 locked coil track rope (LCTR) is essentially composed of wires (round and rail-shaped) laid helically in different layers. These wire ropes are sometimes used in conveyors carrying empty and loaded buckets in mining areas. During service, such wire ropes may fail prematurely due to disintegration/failure of individual groups of wires. To understand the genesis of LCTR wire failures, a detailed metallurgical investigation of failed rope wires was made and included visual examination, optical microscopy, scanning electron microscopy (SEM), and electron probe microanalysis (EPMA). Two types of failed wires were investigated; one is from a 40 mm diameter locked coil track rope and the other from a 53 mm locked coil track rope. Optical microscopy of failed round wires in the 53 mm diameter rope clearly revealed fully decarburized layers at the surface and a few grain-boundary cracks. From the location of the failure, it was clear that apart from static tensile loads, the wire ropes had been subjected to bending and unbending loads near the saddle, as fully loaded or empty buckets traveled access the conveyor. The SEM studies confirmed that the fracture had been caused by initiation of fatigue cracks in the decarburized zone under conditions of repeated bending and unbending stresses superimposed on the static tensile load.

An extensive metallurgical investigation was carried out on samples of a failed roller bearing from the support and tilting system of a basic oxygen furnace converter used in the steel melting shop of an integrated steel plant. The converter bearing was fabricated from low-carbon, carburizing grade steel and had failed in service within a year of fitting to a repaired shaft. Microscopic observations of both the broken roller and inner-race samples revealed subsurface cracking and preponderance of brittle oxide and other macroinclusions. Electron probe microanalysis studies confirmed that the brittle oxides that formed stringers were alumina, and the other macroinclusions were complex silicates. Both the alumina and silicate inclusions were deleterious to contact-fatigue properties. Microstructurally, the carburized regions of the broken roller and of inner-race samples contained high-carbon tempered martensite. Microhardness measurements revealed that. Although the core hardness of the roller and the inner-race samples were similar, the surface hardness of the roller was approximately 8.5 HRC units harder than that of the inner-race. SEM observations of the roller fracture surface revealed striations indicative of fatigue, and EDS analyses corroborated a high incidence of silicate inclusions at crack sites. The study suggests that the failure of the bearing occurred because the hardness difference between the roller bearing and the inner-race surfaces resulted in wear of the inner-race. The wear led to shaft misalignment and play during service. The misalignment, coupled with the presence of inclusions, caused fatigue failure of the roller bearing.

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.

An investigation was conducted to better understand the time-dependent degradation of thermal barrier coated superalloy components in gas turbines. First-stage vanes are normally subjected to the highest gas velocities and temperatures during operation, and were thus the focus of the study. The samples that were analyzed had been operating at 1350 °C in a gas turbine at a combined-cycle generating plant. They were regenerated once, then used for different lengths of time. The investigation included chemical analysis, scanning electron microscopy, SEM/energy dispersive spectroscopy, and x-ray diffraction. It was shown that degradation is driven by chemical and mechanical differences, oxide growth, depletion, and recrystallization, the combined effect of which results in exfoliation, spallation, and mechanical thinning.