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scanning auger microprobe
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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
... 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...
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: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001318
EISBN: 978-1-62708-215-0
... 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...
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.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.aero.c0006402
EISBN: 978-1-62708-217-4
..., H2SO4 anodized, and coated with MIL-C-27725 integral fuel tank coating on the rib side. Scanning electron microscopy and microprobe analysis (both conventional energy-dispersive and Auger analyzers) showed that the anodic coating was applied over an improperly cleaned and contaminated surface...
Abstract
New aircraft wing panels extruded from 7075-T6 aluminum exhibited an unusual pattern of circular black interrupted lines, which could not be removed by scouring or light sanding. The panels, subsequent to profiling and machining, were required to be penetrated inspected, shot peened, H2SO4 anodized, and coated with MIL-C-27725 integral fuel tank coating on the rib side. Scanning electron microscopy and microprobe analysis (both conventional energy-dispersive and Auger analyzers) showed that the anodic coating was applied over an improperly cleaned and contaminated surface. The expanding corrosion product had cracked and, in some places, had flaked away the anodized coating. The corrodent had penetrated the base aluminum in the form of subsurface intergranular attack to a depth of 0.035 mm (0.0014 in.). It was recommended that a vapor degreaser be used during cleaning prior to anodizing. A hot inhibited alkaline cleaner was also recommended during cleaning prior to anodizing. The panels should be dichromate sealed after anodizing. The use of deionized water was also recommended during the dichromate sealing operation. In addition, the use of an epoxy primer prior to shipment of the panels was endorsed. Most importantly, surveillance of the anodizing process itself was emphasized.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.power.c9001676
EISBN: 978-1-62708-229-7
...-dispersive x-ray analysis was performed using a Tracor Northern NS 880 x-ray analyzer attachment. Auger analysis was performed using a Physical Electronics 595 scanning Auger microprobe with a 5 kV electron beam. Results Varying amounts of corrosion were observed along the length of the detector...
Abstract
The self-powered flux detectors used in some nuclear reactors are Pt or V-cored co-axial cables with MgO as an insulator and Inconel 600 as the outer sheath material. The detectors are designed to operate in a He atmosphere; to maximize the conduction of heat (generated from the interaction with gamma radiation) and to prevent corrosion. A number of failures have occurred over the years because of a loss of the He cover gas in the assembly. This has resulted in either acid attack on the Inconel 600 sheath in a wet environment or gaseous corrosion in a dry environment. In the latter case, nitriding and embrittlement occurred at temperatures as low as 300 to 400 deg C (determined from an examination of the oxidation of the Zircaloy-2 carrier rod on which the detectors were mounted). Recent results are described and discussed in terms of the oxidation and nitriding kinetics of Zircaloy-2 and Inconel 600, respectively.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.pulp.c0045911
EISBN: 978-1-62708-230-3
... on the apparently clean fracture areas. This was done using the scanning Auger microscope on several portions of the various fractures. The Auger spectra obtained from one fracture, as received in the laboratory and after argon ion etching for 12 min (equal to about 120 nm), showed that the entire oxide thickness...
Abstract
Within the first few months of operation of an 8 km (5 mile) long 455 mm (18 in.) diam high-pressure steam line between a coal-fired electricity-generating plant and a paper mill, several of the Inconel 600 bellows failed. The steam line operated at 6030 kPa (875 psi) and 420 deg C (790 deg F). Metallographic sections, energy-dispersive x-ray spectra, chemical analyses, tensile tests, and Auger microscope analyses showed the failed bellows met the specifications for the material. However, investigation also showed entire oxide thickness was contaminated with relatively large amounts of sodium, calcium, potassium, aluminum, and sulfur, alkali, alkali earth, and other contaminants that completely permeated even the thin oxides on the fracture surfaces. Additional investigation of the purity of the steam itself as reported by the power plant showed that corrosion and cracks were ultimately caused by the steam. While under normal operation, the steam's purity posed no problem to the material, during boiler cleaning operations, the generating plant had allowed contamination to get into the steam line.
Series: 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
... temperature, FATT, curves were obtained. Small bar samples, 25mm long, 2mm × 2mm, were machined from broken charpy specimens and fractured at liquid nitrogen temperatures in a scanning auger microprobe, SAM. Ten separate grain boundaries were analysed, utilising auger spectroscopy ( 9 ) in each sample...
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.
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
... elements were detected in the grain boundaries. The embrittled tube was then analyzed using an Auger electron scanning microprobe. A notched sample was fractured under ultrahigh vacuum. Tellurium and carbon, along with oxygen, copper, and nickel, were detected on much of the intergranular fracture...
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.a0003520
EISBN: 978-1-62708-180-1
... to analyze inclusions or corrodents observed on the fracture face. A more recently developed tool is the scanning Auger microprobe, which is capable of analyzing surfaces on an atomic scale. This tool is very useful in analyzing surface films and in detecting impurity segregation that causes temper...
Abstract
This article outlines the basic steps to be followed and the range of techniques available for failure analysis, namely, background data assembling, visual examination, microfractography, chemical analysis, metallographic examination, electron microscopy, electron microprobe analysis, X-ray techniques, and simulations. It also describes the steps for analyzing the data, preparing the report, preservation of evidence, and follow-up on recommendations.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006786
EISBN: 978-1-62708-295-2
... detected using scanning Auger microprobe 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...
Abstract
Metal-induced embrittlement is a phenomenon in which the ductility or the fracture stress of a solid metal is reduced by surface contact with another metal in either the liquid or solid form. This article summarizes some of the characteristics of liquid-metal- and solid-metal-induced embrittlement. This phenomenon shares many of these characteristics with other modes of environmentally induced cracking, such as hydrogen embrittlement and stress-corrosion cracking. The discussion covers the occurrence, failure analysis, and service failures of the embrittlement. The article also briefly reviews some commercial alloy systems in which liquid-metal-induced embrittlement or solid-metal-induced embrittlement has been documented and describes some examples of cracking due to these phenomena, either in manufacturing or in service.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003554
EISBN: 978-1-62708-180-1
... indicated that failure occurred intergranularly from the cylinder side. Energy-dispersive spectroscopy analysis indicated the presence of mercury on the fracture surface, and mercury was also detected using scanning Auger microprobe analysis. The mercury was accidentally introduced into the cylinders during...
Abstract
Metal-induced embrittlement is a phenomenon in which the ductility or fracture stress of a solid metal is reduced by surface contact with another metal in either liquid or solid form. This article summarizes the characteristics of solid metal induced embrittlement (SMIE) and liquid metal induced embrittlement (LMIE). It describes the unique features that assist in arriving at a clear conclusion whether SMIE or LMIE is the most probable cause of the problem. The article briefly reviews some commercial alloy systems where LMIE or SMIE has been documented. It also provides some examples of cracking due to these phenomena, either in manufacturing or in service.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006943
EISBN: 978-1-62708-395-9
... 9. Wolstenholme J. , Auger Electron Spectroscopy: Practical Application to Materials Analysis and Characterization of Surfaces, Interfaces, and Thin Films , Momentum Press , LLC, New York , 2015 , p 1 – 10 10. Goldstein J.I. et al. , Cathodoluminescence , Scanning...
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.power.c9001666
EISBN: 978-1-62708-229-7
.... Fig. 13 EDXA concentration profiles within crack, transverse section. After the crack was broken open, deposits on the entire crack surface were analyzed in the SEM and, in addition, with the Auger microprobe. The results confirmed that chlorine was present on the fracture faces but only...
Abstract
Stress-corrosion cracking of low-alloy steel turbine discs has emerged as a generic concern in nuclear generating stations. An investigation that made extensive use of field metallographic techniques to examine suspected cracking in such a component is described. The crack position, and its relationship to surface topographic features, were examined and recorded by magnetic rubber and high-resolution dental rubber replicating materials. Corrosion deposits on keyway surfaces and within the crack were collected with acetate foil replicas applied and then stripped from the keyway surfaces. Microstructural details were revealed by the use of field metallographic preparation techniques and replicated by acetate foil for examination with optical and scanning electron microscopes. It was possible by these techniques to establish the cracking mechanism as stress corrosion possibly related to chloride or sulphate ion steam contaminants. Subsequent sectioning and conventional metallography confirmed both the validity of the conclusions and the replication techniques.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006759
EISBN: 978-1-62708-295-2
... be sampled to later perform chemical analysis using other methods. Electron microprobe analysis or electron probe microanalysis is an alternative to scanning electron microscopy for performing chemical analysis. Electron probe microanalysis in conjunction with WDS is considered more quantitative than...
Abstract
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.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003529
EISBN: 978-1-62708-180-1
... to the application of stress or was caused by a sustained stress. Auger analysis may be used in bigger investigations of more costly failures, to preclude embrittlement of grain boundaries by other low melting point elements, such as sulfur, antimony, tin, and phosphorus. Any of these tests would probably shed more...
Abstract
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.
Book Chapter
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003524
EISBN: 978-1-62708-180-1
... region using acetate tape softened in acetone, dried, then carefully stripped from the fracture surface. Upon return to the laboratory, the replicas may be gold coated and examined with a scanning electron microscope (SEM). Foreign particles removed from the fracture surface also may be analyzed...
Abstract
This article describes the preliminary stages and general procedures, techniques, and precautions employed in the investigation and analysis of metallurgical failures that occur in service. The most common causes of failure characteristics are described for fracture, corrosion, and wear failures. The article provides information on the synthesis and interpretation of results from the investigation. Finally, it presents key guidelines for conducting a failure analysis.
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
Series: 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
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
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006790
EISBN: 978-1-62708-295-2
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.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003553
EISBN: 978-1-62708-180-1
... inspection had included careful scrutiny of all pipe welds by both visual and ultrasonic examination. Following discovery of the two leaks, the entire line of 150 mm (6 in.) pipe, which contained 16 welds, was carefully scanned. Five additional defects were discovered, all circumferential and all in HAZs...
Abstract
This article commences with a discussion on the characteristics of stress-corrosion cracking (SCC) and describes crack initiation and propagation during SCC. It reviews the various mechanisms of SCC and addresses electrochemical and stress-sorption theories. The article explains the SCC, which occurs due to welding, metalworking process, and stress concentration, including options for investigation and corrective measures. It describes the sources of stresses in service and the effect of composition and metal structure on the susceptibility of SCC. The article provides information on specific ions and substances, service environments, and preservice environments responsible for SCC. It details the analysis of SCC failures, which include on-site examination, sampling, observation of fracture surface characteristics, macroscopic examination, microscopic examination, chemical analysis, metallographic analysis, and simulated-service tests. It provides case studies for the analysis of SCC service failures and their occurrence in steels, stainless steels, and commercial alloys of aluminum, copper, magnesium, and titanium.