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Book Chapter
X-Ray Spectroscopy in Failure Analysis
Available to PurchaseSeries: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006770
EISBN: 978-1-62708-295-2
.... Thus, x-ray spectroscopy is simply the manner by which this spectrum of x-rays is produced. Note that this spectrum is limited at both the low and high ends of the energy/wavelength scale. Because it takes energy to remove an electron from its orbital and cause it to be ejected from the atom, the high...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001335
EISBN: 978-1-62708-215-0
.... Discussion Many polycrystalline metals can become brittle and fail along grain boundaries when a low stress is applied. The brittleness has been attributed to intergranular weakness caused by the precipitation or segregation of impurities to grain boundaries. For example, Auger electron spectroscopy...
Abstract
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.
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
..., which provide a topographic view of the sample by detecting low-energy electrons emitted from the surface, are used to locate specific areas for more detailed study. Backscattered electron images, involving higher-energy electrons that have undergone scattering processes before escaping from the sample...
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.
Book Chapter
Chemical Characterization of Surfaces
Available to PurchaseSeries: 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 topographic view of the sample by detecting low-energy electrons emitted from the surface, are used to locate specific areas for more detailed study. The BSE images, involving higher-energy electrons that have undergone scattering processes before escaping from the sample, reveal atomic number contrast...
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.
Book Chapter
Failure Analysis of a Set of 1CrMoV Studs From a Steam Turbine and Techniques for Its Assessment
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.power.c9001004
EISBN: 978-1-62708-229-7
... as a % of a monolayer. At low energy values, the data scatter became a limiting factor in the assessment. However, at such values the material was severely embrittled and the data scatter was much less in the practically important regime, i.e., the transition region. The EPR results, however, were disappointing...
Abstract
The results of a failure analysis of a series of Cr-Mo-V steel turbine studs which had experienced a service lifetime of some 50,000 h are described. It was observed that certain studs suffered complete fracture while others showed significant defects located at the first stress bearing thread. Crack extension was the result of marked creep embrittlement and reverse temper embrittlement (RTE). Selected approaches were examined to assess the effects of RTE on the material toughness of selected studs. It was observed that Auger electron microscopy results which indicated the extent of grain boundary phosphorus segregation exhibited a good relationship with ambient temperature Charpy data. The electrochemical polarization kinetic reactivation, EPR, approach, however, proved disappointing in that the overlapping scatter in the minimum current density, Ir, for an embrittled and a non-embrittled material was such that no clear decision of the toughness properties was possible by this approach. The initial results obtained from small punch testing showed good agreement with other reported data and could be related to the FATT. Indeed, this small punch test, combined with a miniature sample sampling method, represents an attractive approach to the toughness assessment of critical power plant components.
Book Chapter
Surface Examination and Analysis of Plastics
Available to PurchaseSeries: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006943
EISBN: 978-1-62708-395-9
... results in one or more of the inner electrons being knocked out to a higher electron shell. Spectroscopy is based on the ability of the incident electron to eject a core electron from the atom and the direct relationship between the energy of the photon released with the atomic number. The atom deexcites...
Abstract
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.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006931
EISBN: 978-1-62708-395-9
... spectroscopy Mass/charge of ions produced Molecular structure X-ray diffraction analysis (XRD) Crystalline polymer component Crystalline structure, short- and long-range ordering, percent crystallinity, polymer blend/copolymer Small-angle x-ray diffraction X-ray scattering at low angle Crystallite...
Abstract
This article presents tools, techniques, and procedures that engineers and material scientists can use to investigate plastic part failures. It also provides a brief survey of polymer systems and the key properties that need to be measured during failure analysis. It describes the characterization of plastics by infrared and nuclear magnetic resonance spectroscopy, differential scanning calorimetry, differential thermal analysis, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The article also discusses the use of X-ray diffraction for analyzing crystal phases and structures in solid materials.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003522
EISBN: 978-1-62708-180-1
...) spectroscopy Chemical shift of nuclei Mass spectroscopy Mass/charge of ions produced X-ray diffraction analysis (XRD) Crystalline polymer component Small-angle x-ray diffraction X-ray scattering at low angle Scanning electron microscopy (SEM) Surface and particle morphology Transmission...
Abstract
This article focuses on the visual or macroscopic examination of damaged materials and interpretation of damage and fracture features. Analytical tools available for evaluations of corrosion and wear damage features include energy dispersive spectroscopy, electron probe microanalysis, Auger electron spectroscopy, secondary ion mass spectroscopy, and X-ray powder diffraction. The article discusses the analysis and interpretation of base material composition and microstructures. Preparation and examination of metallographic specimens in failure analysis are also discussed. The article concludes with a review of the evaluation of polymers and ceramic materials in failure analysis.
Book Chapter
Scanning Electron Microscopy for Failure Analysis
Available to PurchaseSeries: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006769
EISBN: 978-1-62708-295-2
... as a function of atomic number Due to their low energy, secondary electrons are typically attracted to a photomultiplier/scintillator detector by placing a positive bias on the detector. For each pixel where the beam interacts with the sample, a signal is collected, processed, and displayed...
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.
Book Chapter
Examination of Damage and Material Evaluation
Available to PurchaseSeries: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006757
EISBN: 978-1-62708-295-2
... (NMR) spectroscopy Chemical shift of nuclei Mass spectroscopy Mass/charge of ions produced X-ray diffraction analysis (XRD) Crystalline polymer component Small-angle x-ray diffraction X-ray scattering at low angle Scanning electron microscopy (SEM) Surface and particle morphology...
Abstract
Examination of a damaged component involves a chain of activities that, first and foremost, requires good observation and documentation. Following receipt and documentation, the features of damage can be recorded and their cause(s) investigated, as this article briefly describes, for typical types of damage experienced for metallic components. This article discusses the processes involved in visual or macroscopic examination of damaged material; the interpretation of fracture features, corrosion, and wear damage features; and the analysis of base material composition. It covers the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed.
Book Chapter
Photochemical Aging and Weathering of Polymers—The Basics
Available to PurchaseSeries: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006920
EISBN: 978-1-62708-395-9
... molecule typically releases the energy in the form of a photon (fluorescence or phosphorescence) or in the form of heat and falls back into its ground state without any damage. However, the excited chromophore may have sufficient energy for bond dissociation or to abstract a hydrogen atom from the polymer...
Abstract
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.
Book
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.9781627083959
EISBN: 978-1-62708-395-9
Book Chapter
Fundamentals of Polymer Additives
Available to PurchaseSeries: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006939
EISBN: 978-1-62708-395-9
... modifier; they are broadly divided into three categories based on critical information provided by the analyses. Chemical Nature Organic and inorganic surface modifiers can be characterized by using spectroscopy (ultraviolet-visible, infrared, nuclear magnetic resonance) and x-ray based (energy...
Abstract
Polymer materials are key building blocks of the modern world, commonly used in packaging, automobiles, building materials, electronics, telecommunications, and many other industries. These commercial applications of polymeric materials would not be possible without the use of additives. This article is divided into five sections: mechanical property modifiers, physical property modifiers, biological function modifiers, processing aids, and colorants. It describes three classes of additives that are used to inhibit biological activity, six classes of mechanical property modifiers, three classes of physical property modifiers, and two classes of both colorants and processing aids.
Book Chapter
Failures of Structures and Components by Metal-Induced Embrittlement
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001812
EISBN: 978-1-62708-241-9
..., but in general the composition of any deposits can be determined by Energy-Dispersive Spectroscopy (EDS) or by other techniques. For SMIE, embrittling metal films on fracture surfaces are also sometimes evident from their colour, e.g. for copper and oxidized cadmium, but are often not obvious even using high...
Abstract
Several cases of embrittlement failure are analyzed, including liquid-metal embrittlement (LME) of an aluminum alloy pipe in a natural gas plant, solid metal-induced embrittlement (SMIE) of a brass valve in an aircraft engine oil cooler, LME of a cadmium-plated steel screw from a crashed helicopter, and LME of a steel gear by a copper alloy from an overheated bearing. The case histories illustrate how LME and SMIE failures can be diagnosed and distinguished from other failure modes, and shed light on the underlying causes of failure and how they might be prevented. The application of LME as a failure analysis tool is also discussed.
Book Chapter
Hot Corrosion of Stainless Steel Grate Bars in Taconite Indurators
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001109
EISBN: 978-1-62708-214-3
... bars that had spent 9 months in service were dipped and rinsed in distilled water containing 1% HNO 3 in order to extract water-soluble salts from the corrosion products. Chemical analysis of the solution, using atomic absorption spectroscopy and ion-exchange chromatography, yielded Na K + , Ca 2...
Abstract
Grate bars in the traveling grate indurators in several taconite processing units suffered excessive corrosion following a conversion from acid to fluxed pellet production procedures. The campaign life of the HH grade cast stainless steel bars was reduced from more than 7 years to approximately 9 months. Several corroded grate bars were examined metallographically and by electron microscopy to determine the causes of the accelerated corrosion. Chemical and X-ray diffraction analyses were also conducted, along with simulation tests to assess the role of alkali chlorides in the corrosion process. The basic cause of degradation was found to be hot corrosion caused by the deposition of alkali sulfates and chlorides. However this degradation may have been aggravated by thermal cycling and abrasion. The source of the salt was impurities in the flux. Two potential solutions were proposed: modification of the processing parameters to reduce the salt deposition and / or change of bar materials to a more resistant alloy.
Book Chapter
High-Temperature Corrosion-Related Failures
Available to PurchaseSeries: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006787
EISBN: 978-1-62708-295-2
... saturation concentration is attained. Lowering the pH increases the hydrogen saturation concentration slightly, but it greatly increases the adsorption rate of atomic hydrogen, which can explain why low-pH conditions lead to hydrogen damage in shorter exposure times. The presence of diffusible atomic...
Abstract
High-temperature corrosion can occur in numerous environments and is affected by various parameters such as temperature, alloy and protective coating compositions, stress, time, and gas composition. This article discusses the primary mechanisms of high-temperature corrosion, namely oxidation, carburization, metal dusting, nitridation, carbonitridation, sulfidation, and chloridation. Several other potential degradation processes, namely hot corrosion, hydrogen interactions, molten salts, aging, molten sand, erosion-corrosion, and environmental cracking, are discussed under boiler tube failures, molten salts for energy storage, and degradation and failures in gas turbines. The article describes the effects of environment on aero gas turbine engines and provides an overview of aging, diffusion, and interdiffusion phenomena. It also discusses the processes involved in high-temperature coatings that improve performance of superalloy.
Book Chapter
Failures of Pipelines
Available to PurchaseSeries: ASM Handbook
Volume: 11A
Publisher: ASM International
Published: 30 August 2021
DOI: 10.31399/asm.hb.v11A.a0006822
EISBN: 978-1-62708-329-4
... the chemical composition of surface residue. Various techniques may be used, including energy-dispersive spectroscopy, x-ray diffraction, or gas chromatography/mass spectrometry. Where microbiologically influenced corrosion is suspected as a possible cause or contributor to a failure, deposit samples should...
Abstract
This article discusses the failure analysis of several steel transmission pipeline failures, describes the causes and characteristics of specific pipeline failure modes, and introduces pipeline failure prevention and integrity management practices and methodologies. In addition, it covers the use of transmission pipeline in North America, discusses the procedures in pipeline failure analysis investigation, and provides a brief background on the most commonly observed pipeline flaws and degradation mechanisms. A case study related to hydrogen cracking and a hard spot is also presented.
Book Chapter
Abrasive Wear Failures
Available to PurchaseSeries: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003560
EISBN: 978-1-62708-180-1
..., dislocations easily cross slip. The rate of cross slip for a given alloy or element is usually indicated by its stacking-fault energy. Dislocation cross slip is hindered by the presence of stacking faults, and a high stacking-fault energy indicates a low number of impeding stacking faults and an increased...
Abstract
Wear, a form of surface deterioration, is a factor in a majority of component failures. This article is primarily concerned with abrasive wear mechanisms such as plastic deformation, cutting, and fragmentation which, at their core, stem from a difference in hardness between contacting surfaces. Adhesive wear, the type of wear that occurs between two mutually soluble materials, is also discussed, as is erosive wear, liquid impingement, and cavitation wear. The article also presents a procedure for failure analysis and provides a number of detailed examples, including jaw-type rock crusher wear, electronic circuit board drill wear, grinding plate wear failure analysis, impact wear of disk cutters, and identification of abrasive wear modes in martensitic steels.
Book Chapter
Abrasive Wear Failures
Available to PurchaseSeries: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006790
EISBN: 978-1-62708-295-2
.... Dislocation cross slip is hindered by the presence of stacking faults, and a high stacking-fault energy indicates a low number of impeding stacking faults and an increased tendency to cross slip and hence gall. Nickel and aluminum have poor galling resistance, whereas gold and copper have good galling...
Abstract
Engineered components fail predominantly in four major ways: fracture, corrosion, wear, and undesirable deformation (i.e., distortion). Typical fracture mechanisms feature rapid crack growth by ductile or brittle cracking; more progressive (subcritical) forms involve crack growth by fatigue, creep, or environmentally-assisted cracking. Corrosion and wear are another form of progressive material alteration or removal that can lead to failure or obsolescence. This article primarily covers the topic of abrasive wear failures, covering the general classification of wear. It also discusses methods that may apply to any form of wear mechanism, because it is important to identify all mechanisms or combinations of wear mechanisms during failure analysis. The article concludes by presenting several examples of abrasive wear.
Book Chapter
Fracture Appearance and Mechanisms of Deformation and Fracture
Available to PurchaseSeries: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006774
EISBN: 978-1-62708-295-2
... compressive hydrostatic component relative to the deviatoric component of stress and decreases with an increase in the tensile-hydrostatic stress component. It is also possible for ductile fracture to require little energy for initiation or propagation if strain-hardening capacity is low. From...
Abstract
Engineering component and structure failures manifest through many mechanisms but are most often associated with fracture in one or more forms. This article introduces the subject of fractography and aspects of how it is used in failure analysis. The basic types of fracture processes (ductile, brittle, fatigue, and creep) are described briefly, principally in terms of fracture appearances. A description of the surface, structure, and behavior of each fracture process is also included. The article provides a framework from which a prospective analyst can begin to study the fracture of a component of interest in a failure investigation. Details on the mechanisms of deformation, brittle transgranular fracture, intergranular fracture, fatigue fracture, and environmentally affected fracture are also provided.
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