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Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006771
EISBN: 978-1-62708-295-2
... A.J. , and Sano N. , Accurate Argon Cluster-Ion Sputter Yields: Measured Yields and Effect of the Sputter Threshold in Practical Depth-Profiling by X-Ray Photoelectron Spectroscopy and Secondary Ion Mass Spectrometry , J. Appl. Phys. , Vol 114 , 2013 10.1063/1.4823815 12. Douglas...
Abstract
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.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003534
EISBN: 978-1-62708-180-1
..., when excessive atmospheric or handling contamination obscures much of the underlying surface of interest, inert gas sputtering can be employed to remove at least some of the obstructing contamination layer. Care must be taken to prevent sputter removing too much of the sample, or the surface...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001833
EISBN: 978-1-62708-241-9
... for calculation. Grain boundaries and cleavage planes on the fracture surface were selected for depth profiling. The sputter rate was estimated according to the method recommended in Ref 1 . Chemical Composition of Steam Chest Material (wt.%) Table 1 Chemical Composition of Steam Chest Material (wt...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001752
EISBN: 978-1-62708-241-9
... of iron-nitrogen-boron-carbon ( Fig. 9 ) and some oxygen even after the spherical surface was argon gas “sputtered” (ion etched) to remove 10–15 atom layers of surface ( Table 2 ). Some manganese sulfide particles are in adjacent dimples on the same planar dimpled facet. Fig. 8 SEM micrograph shows...
Abstract
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.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003563
EISBN: 978-1-62708-180-1
... over several hundred-million cycles without failure. These investigations indicate that the RCF performance of nitride (especially TiN and HfN) and DLC coatings can easily outperform conventional bearing materials, whereas other coating materials such as CrN show a promise for the future. Sputtering...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c9001628
EISBN: 978-1-62708-234-1
... the surface being analyzed. X-ray photoelectron spectroscopy measures the binding energies of the elements on the sample surface and is useful for characterizing the elements that are present on the surface, as well as determining the oxidation state of these elements. Furthermore, a sputtering technique...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.process.c9001629
EISBN: 978-1-62708-235-8
... from the surface and also has the effect of implanting the primary ions into the surface. The nature of this technique makes it feasible for analyzing trace amounts of substances; however, extensive knowledge of the sputtering rate is needed in conjunction with calibration of the obtained signals...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c9001516
EISBN: 978-1-62708-234-1
... is then sputtered by physical vapor deposition process or electrolytically or electroless deposited. In order to protect this magnetic film, which stores the data, a thin carbon film is sputtered. The carbon film acts both as a protective film and lubricant. The carbon overcoat, in its turn, protected...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001038
EISBN: 978-1-62708-214-3
... be performed. The replicated tape specimens were sputter coated with 60Au-40Pd for SEM examination. All of the areas were scanned at varying magnifications. Special emphasis was placed on locations 6, 7, and 9, where possible fatigue initiation points had been observed ( Fig. 2 , 3 , 4 ). Fig. 2...
Abstract
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.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003533
EISBN: 978-1-62708-180-1
... and sputter coating. Evaporation coating consists of heating a metal filament to a high temperature in a vacuum chamber to cause evaporation to occur. Atoms that leave the filament travel a line-of-sight trajectory to the surface of the sample where they are adsorbed. A thin coating consisting of a few...
Abstract
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.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003539
EISBN: 978-1-62708-180-1
..., such as carbon or a metal, to allow examination using a standard SEM. The coating is applied by a method such as vacuum evaporation or sputtering. Coating must be performed carefully to avoid damaging the fracture surface (e.g., by excessive heating) or introducing artifacts associated with the coating process...
Abstract
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.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006769
EISBN: 978-1-62708-295-2
... graphite or silver particles. Conductive paint is commercially available from various manufacturers and suppliers. If a nonconductive sample is to be examined using a conventional SEM, several methods exist to produce a conductive layer on the surface. The two most common are evaporation and sputter...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001767
EISBN: 978-1-62708-241-9
... for evaluation at high magnification and with great depth of field. Prior to examination, the fracture surface was cleaned and subsequently gold sputter coated. A review of the fracture surface supported multiple origins at the transformer side of the bracket. These origins extended via a cyclic mechanism...
Abstract
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.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006776
EISBN: 978-1-62708-295-2
... platinum sputter coating of a 4.6 mm (0.18 in.) diameter polycarbonate rotating-beam fatigue specimen. This scanning electron microscope view shows a pattern in the coating reminiscent of “mud-cracking.” Fig. 49 Scanning electron microscope view of fatigue striations in medium-density...
Abstract
Fatigue failure of engineering components and structures results from progressive fracture caused by cyclic or fluctuating loads. Fatigue is an important potential cause of mechanical failure, because most engineering components or structures are or can be subjected to cyclic loads during their lifetime. This article focuses on fractography of fatigue. It provides an abbreviated summary of fatigue processes and mechanisms: fatigue crack initiation, fatigue crack propagation, and final fracture,. Characteristic fatigue fracture features that can be discerned visually or under low magnification are then described. Typical microscopic features observed on structural metals are presented subsequently, followed by a brief discussion on fatigue in polymers and polymer-matrix composites.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001803
EISBN: 978-1-62708-241-9
.... , Van der Waerden J.P. , and deGroot K. : “ Application of Magnetron Sputtering for Producing Ceramic Coatings on Implant Materials ,” Clin. Oral Implants Res. , 1993 , 4 , pp. 28 – 34 10.1034/j.1600-0501.1993.040104.x . 9. Kim C.S. and Ducheyne P. : “ Compositional...
Abstract
Metallurgical SEM analysis provides many insights into the failure of biomedical materials and devices. The results of several such investigations are reported here, including findings and conclusions from the examination a total hip prosthesis, stainless steel and titanium compression plates, and hollow spinal rods. Some of the failure mechanisms that were identified include corrosive attack, corrosion plus erosion-corrosion, inclusions and stress gaps, production impurities, design flaws, and manufacturing defects. Failure prevention and mitigation strategies are also discussed.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001269
EISBN: 978-1-62708-215-0
.... 50×. Fig. 8 Energy dispersive spectra showing titanium and nitrogen on the surface. Sample after gold sputter coating. 500×. Hardness Hardness readings taken in accordance with ASTM E18-89 indicate the bulk/core hardness to be 64 HRC. Knoop readings were taken in accordance...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001318
EISBN: 978-1-62708-215-0
... elements found that were extraneous to the findings on a disc that had not been exposed to the gas blend. Since the minimum XPS analysis area of 4 mm 2 (0.016 in. 2 ) was inappropriate for analysing the narrow fracture surface of the failed discs, SAM was used. After ion sputtering to remove carbon...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.bldgs.c9001528
EISBN: 978-1-62708-219-8
... of the chlorides responsible for TGSCC and corrosion of the tank OD. Fig. 6 EDS chemical analysis of the black foam insulation reveals a high level of chlorine. Sample is sputter-coated with gold. Circumferential and axial cross sections were metallographically prepared for examination of crack...
Abstract
A 5000-gal (20,000-L) hot-water holding tank fractured at a large automotive manufacturing plant. The tank was made from Type 304 austenitic stainless steel. The inner diameter of the tank displayed a macroscopic, web-like network of cracks that deceptively suggested intergranular stress-corrosion cracking. The problem, however, originated on the outside surface of the tank where a tensile stress (due to low applied stress and fabrication-induced residual stresses) accelerated the growth of numerous stress corrosion cracks that eventually broke through to the inner surface, causing leakage and ultimately failure.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001385
EISBN: 978-1-62708-215-0
... off by the homeowner. Molten aluminum at approximately 593 °C (1100 °F) sputtered out of the service panel and ignited combustibles located on the floor below. Improper tightening was also the most probable cause in incident 3 and may have contributed to incident 2 as well. However, water ingress...
Abstract
Three instances involving the failure of aluminum wiring at the service entrance to single-family homes are discussed. Arcing led to a fire which severely damaged a home in one case. In a second, the failure sequence was initiated by water intrusion into the service entrance electrical box during construction of the home. In the third, failure was caused by a marginal installation. Strict adherence to all applicable electrical codes and standards is critical in the case of aluminum wiring. Electrical components not specifically designed for aluminum must never be used with this type of wiring. All doors, panels and similar portions of electrical boxes should be secured to prevent damage to surroundings in the event of an electrical fault. If symptoms of arcing are observed, professional service should be sought. The latest designs of connectors for use with aluminum wiring are less susceptible to deviations in installation practice.
Book Chapter
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001769
EISBN: 978-1-62708-241-9
...) and then immersed in 0.1 M sodium cacodylate buffer (pH 7.2). The coupons were dehydrated using different concentration of ethanol solution 25%, 50%, 75%, and 100% concentration. The air-dried coupons were sputter coated with gold using ion sputters. The coupons were examined at different magnifications [2.0, 5.0...
Abstract
This study examines the role of calcium-precipitating bacteria (CPB) in heat exchanger tube failures. Several types of bacteria, including Serratia sp. (FJ973548), Enterobacter sp. (FJ973549, FJ973550), and Enterococcus sp. (FJ973551), were found in scale collected from heat exchanger tubes taken out of service at a gas turbine power station. The corrosive effect of each type of bacteria on mild steel was investigated using electrochemical (polarization and impedance) techniques, and the biogenic calcium scale formations analyzed by XRD. It was shown that the bacteria contribute directly to the formation of calcium carbonate, a critical factor in the buildup of scale and pitting corrosion on heat exchanger tubes.