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electron-dispersive x-ray analysis
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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.c9001761
EISBN: 978-1-62708-241-9
... electron microscope (SEM) equipped with electron-dispersive X-ray analysis (EDAX). Microhardness gradient through the nitrided layer close to fracture, surface hardness, and macrohardness at the journals were all measured. Fractographic analysis indicated that fatigue was the dominant mechanism of failure...
Abstract
An investigation of a damaged crankshaft from a horizontal, six-cylinder, in-line diesel engine of a public bus was conducted after several failure cases were reported by the bus company. All crankshafts were made from forged and nitrided steel. Each crankshaft was sent for grinding, after a life of approximately 300,000 km of service, as requested by the engine manufacturer. After grinding and assembling in the engine, some crankshafts lasted barely 15,000 km before serious fractures took place. Few other crankshafts demonstrated higher lives. Several vital components were damaged as a result of crankshaft failures. It was then decided to send the crankshafts for laboratory investigation to determine the cause of failure. The depth of the nitrided layer near fracture locations in the crankshaft, particularly at the fillet region where cracks were initiated, was determined by scanning electron microscope (SEM) equipped with electron-dispersive X-ray analysis (EDAX). Microhardness gradient through the nitrided layer close to fracture, surface hardness, and macrohardness at the journals were all measured. Fractographic analysis indicated that fatigue was the dominant mechanism of failure of the crankshaft. The partial absence of the nitrided layer in the fillet region, due to over-grinding, caused a decrease in the fatigue strength which, in turn, led to crack initiation and propagation, and eventually premature fracture. Signs of crankshaft misalignment during installation were also suspected as a possible cause of failure. In order to prevent fillet fatigue failure, final grinding should be done carefully and the grinding amount must be controlled to avoid substantial removal of the nitrided layer. Crankshaft alignment during assembly and proper bearing selection should be done carefully.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001326
EISBN: 978-1-62708-215-0
... the axes. SEM examination revealed the presence of longitudinally oriented nonmetallic inclusions that were partly retained and partly dislodged. Electron-dispersive x-ray analysis indicated that the inclusions were composed of CaO. Based on the overall chemistry of the inclusion sites, the source...
Abstract
Pressure testing of a batch of AISI type 316L stainless steel thermowells intended for use in a nuclear power-plant resulted in the identification of leakage at the tips in 20% of the parts. Radiography at the tip region of representative thermowells showed linear indications along the axes. SEM examination revealed the presence of longitudinally oriented nonmetallic inclusions that were partly retained and partly dislodged. Electron-dispersive x-ray analysis indicated that the inclusions were composed of CaO. Based on the overall chemistry of the inclusion sites, the source of the CaO was determined to be slag entrapment during the steel making process. It was recommended that the thermowell blanks be ultrasonically tested prior to machining and that the design be modified to make internal pressurization possible.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006770
EISBN: 978-1-62708-295-2
.... The article ends with a discussion on the applications of x-ray spectroscopy in failure analysis. energy-dispersive spectrometers failure analysis handheld X-ray fluorescence analysis instrumentation scanning electron microscope wavelength-dispersive spectrometers X-ray spectroscopy X-RAY...
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 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 (EDS), electron probe microanalysis (EPMA), Auger electron spectroscopy (AES), secondary ion mass spectroscopy (SIMS), and x-ray powder diffraction (XRPD). Energy-Dispersive X-Ray Analysis Energy-dispersive x-ray analysis is normally conducted using a SEM fitted with an x-ray detector...
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.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.aero.c9001906
EISBN: 978-1-62708-217-4
... testing, scanning electron microscopy, and energy-dispersive x-ray spectroscopy. It was determined that the failures were due to forging defects. Both forging laps and seams acted as stress concentrators when the lugs were loaded during proof testing. Bombs (weapons) Suspension lugs Forging...
Abstract
Suspension lugs fabricated from AISI 4340 steel used to facilitate loading of bombs onto the underside of military aircraft could not sustain required loads during routine proof load testing. Three failed lugs underwent visual examination, chemical analysis, metallography, hardness testing, scanning electron microscopy, and energy-dispersive x-ray spectroscopy. It was determined that the failures were due to forging defects. Both forging laps and seams acted as stress concentrators when the lugs were loaded during proof testing.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001829
EISBN: 978-1-62708-241-9
...-stage vanes, the authors used a scanning electron microscope (SEM) at 20 kV. They then used a SEM-energy dispersive spectroscopy (EDS) method to determine the chemical compositions of specimens. To identify phases, they conducted x-ray diffraction experiments by using a diffractometer with Cu K α...
Abstract
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.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001839
EISBN: 978-1-62708-241-9
... Abstract Several stainless steel coils cracked during a routine unwinding procedure, prompting an investigation to determine the cause. The analysis included optical and scanning electron microscopy, energy-dispersive x-ray spectrometry, and tensile testing. An examination of the fracture...
Abstract
Several stainless steel coils cracked during a routine unwinding procedure, prompting an investigation to determine the cause. The analysis included optical and scanning electron microscopy, energy-dispersive x-ray spectrometry, and tensile testing. An examination of the fracture surfaces revealed a brittle intercrystalline mode of fracture with typical manifestations of clear grain facets. Branched and discrete stepwise microcracks were also found along with unusually high levels of residual hydrogen. Mechanical tests revealed a marked loss of tensile ductility in the defective steel with elongations barely approaching 8%, compared to 50% at the time of delivery weeks earlier. Based on the timing interval and the fact that failure occurred at operating stresses well below the yield point of the material, the failure is being attributed to hydrogen-induced damage. Potential sources of hydrogen are considered as are remedial measures for controlling hydrogen content in steels.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001359
EISBN: 978-1-62708-215-0
... bead of metal sticking to the blade surface in each case. Scanning electron microscope revealed that the cracks initiated at the point of contact of the bead with the blade surface. Energy-dispersive X-ray analysis indicated that the bead composition was the same as that of the blade. Detailed...
Abstract
The cause of low fatigue life measurements obtained during routine fatigue testing of IMI 550 titanium alloy compressor blades used in the first stage of the high-pressure compressor of an aeroengine was investigated. The origin of the fatigue cracks was associated with a spherical bead of metal sticking to the blade surface in each case. Scanning electron microscope revealed that the cracks initiated at the point of contact of the bead with the blade surface. Energy-dispersive X-ray analysis indicated that the bead composition was the same as that of the blade. Detailed investigation revealed that fused material from the blade had been thrown onto the cold blade surface during a grinding operation to remove the targeting bosses from the forgings, thereby causing local embrittlement. It was recommended that extreme care be taken during grinding operations to prevent the hot, fused particles from striking the blade surface.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.med.c0048400
EISBN: 978-1-62708-226-6
... a tension band fixation containing a cerclage wire, two screws, and washers beneath the screw heads. See also Fig. 2 . Fig. 2 Intercrystalline corrosion of a type 304 stainless steel cerclage wire. (a) Broken cerclage wire. (b) Energy-dispersive x-ray analysis under the scanning electron...
Abstract
Cerclage wire, which was used with two screws and washers for a tension band in a corrective internal fixation, was found broken at several points and corroded after nine months in service. The material was examined using energy-dispersive x-ray analysis and determined not to be in compliance with standards (type 304 stainless steel without molybdenum). The screws and washers were found to be made of remelted implant-quality type 316L stainless steel and were intact. Signs of sensitization, characterized by chromium carbide precipitates at the grain boundaries, were revealed by the microstructure. Intercrystalline corrosion with pitted grains was indicated by SEM fractography. Improper heat treatment of the steel was interpreted to have led to intercrystalline corrosion and implant separation.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.homegoods.c9001622
EISBN: 978-1-62708-222-8
...) failure A stamped coin exhibited visible discolored areas, seen as a tan haze on the surface ( Fig. 1 ). In this case, the discoloration was considered merely cosmetic. The nonstained and stained regions were studied using a scanning electron microscope equipped with an energy-dispersive X-ray...
Abstract
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.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c0006417
EISBN: 978-1-62708-234-1
... stainless steel was also recommended. Cadmium plating Corrosion prevention Corrosion products Energy dispersive x ray analysis Inhibitors Iron oxides Materials substitution Pipe bends Scanning electron microscopy 4340 UNS G43400 (Other, general, or unspecified) corrosion A cadmium...
Abstract
A cadmium-plated 4340 Ni-Cr-Mo steel ballast elbow assembly was submitted for failure analysis to determine the element or radical present in an oxidation product found inside the elbow assembly. Energy-dispersive x-ray analysis in the SEM showed that iron was the predominant species, presumably in an oxide form. The inside surface had the appearance of typical corrosion products. Hardness measurements indicated that the 4340 steel was heat treated to a strength of approximately 862 MPa (125 ksi). It was concluded that the oxide detected on the ballast elbow was iron oxide. The possibility that the corrosion products would eventually create a blockage of the affected hole was great considering the small hole diameter (4.2 mm, or 0.165 in.). It was recommended that a quick fix to stop the corrosion would be to apply a corrosion inhibitor inside the hole. This, however, would cause the possibility of inhibitor buildup and the eventual clogging of the hole. A change in the manufacturing process to include a cadmium plating on the hole inside surface was recommended. This was to be accomplished in accordance with MIL specification QQ-P-416, Type II, Class 1. A material change to 300-series stainless steel was also recommended.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.steel.c9001535
EISBN: 978-1-62708-232-7
.... Microstructural issues influencing roll quality, such as characteristics of carbides, tempered martensite, retained austenite, etc., have been extensively studied through optical and scanning electron microscopy, electron-probe microanalysis, image analysis, and x-ray diffractometry. These are discussed...
Abstract
Although a precise understanding of roll failure genesis is complex, the microstructure of a broken roll can often unravel intrinsic deficiencies in material quality responsible for its failure. This is especially relevant in circumstances when, even under a similar mill-operating environment, the failure involves a particular roll or a specific batch of rolls. This paper provides a microstructural insight into the cause of premature breakage of a second-intermediate Sendzimir mill drive roll used at a stainless steel sheet rolling plant under the Steel Authority of India Limited. Microstructural issues influencing roll quality, such as characteristics of carbides, tempered martensite, retained austenite, etc., have been extensively studied through optical and scanning electron microscopy, electron-probe microanalysis, image analysis, and x-ray diffractometry. These are discussed to elucidate specific microstructural inadequacies that accentuated the failure. The study reveals that even through retained austenite content is low (6.29 vol%) and martensite is non-acicular, the roll breakage is a consequence of intergranular cracking caused by improper carbide morphology and distribution.
Image
Published: 15 May 2022
Fig. 1 Depth of analysis, depth of profiling, and length scale presentation in surface examination and analysis of polymers. AFM, atomic force microscopy; SEM, scanning electron microscopy; XPS, x-ray photoelectron spectroscopy; ToF-SIMS, time-of-flight secondary ion mass spectrometry; EDS
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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
... and any other facets of the techniques that would not be known by the customer. Surface Chemical Analysis Failure investigations where the surface of the subject part is important can include surface chemical analysis techniques such as x-ray photoelectron spectroscopy (XPS), or electron...
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.a0003534
EISBN: 978-1-62708-180-1
...: EDS, energy-dispersive spectroscopy; WDS, wavelength-dispersive spectroscopy; AES, Auger electron spectroscopy; XPS, x-ray photoelectron spectroscopy; TOF-SIMS, time-of-flight secondary ion mass spectrometry; FTIR, Fourier transform infrared (spectroscopy) Understanding the various analytical...
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: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001109
EISBN: 978-1-62708-214-3
... sulfides (light gray), in addition to the expected carbides. Electron-dispersive X-ray analysis (EDXA) of the external oxide scale showed considerable variation in the proportions of iron and chromium. The example in Fig. 4 showed that the outer portion was chromium rich, whereas the inner portion...
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.
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
... product on a fracture surface should generally be confined to the strictly qualitative mode. Interpreting the quantitative results from such a test would be very difficult at best. Wavelength-Dispersive Spectrometry Microchemical Analysis In modern x-ray microanalysis, the analyst actually has...
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.
Image
in Intercrystalline Corrosion on Cerclage Wire of Sensitized 304 Type Stainless Steel
> ASM Failure Analysis Case Histories: Medical and Biomedical Devices
Published: 01 June 2019
Fig. 2 Intercrystalline corrosion of a type 304 stainless steel cerclage wire. (a) Broken cerclage wire. (b) Energy-dispersive x-ray analysis under the scanning electron microscope. Lower spectrum: reference material type 316L screw material. Upper spectrum: type 304 steel with less nickel
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Image
Published: 01 January 2002
Fig. 10 Intercrystalline corrosion of a type 304 stainless steel cerclage wire. (a) Broken cerclage wire. (b) Energy-dispersive x-ray analysis under the scanning electron microscope. Lower spectrum: reference material type 316L screw material. Upper spectrum: type 304 steel with less nickel
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Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.9781627081801
EISBN: 978-1-62708-180-1
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