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electron probe X-ray microanalysis
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Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c0046981
EISBN: 978-1-62708-218-1
.... Analysis (visual inspection, electron probe x-ray microanalysis, hardness testing, 4.5x fractograph) supported the conclusions that failure of the valve stem occurred by fatigue as a result of a combination of a nonuniform bending load, which caused a mild stress-concentration condition, and a high...
Abstract
The exhaust valve of a truck engine failed after 488 h of a 1000 h laboratory endurance test. The valve was made of 21-2 valve steel in the solution treated and aged condition and was faced with Stellite 12 alloy. The failure occurred by fracture of the underhead portion of the valve. Analysis (visual inspection, electron probe x-ray microanalysis, hardness testing, 4.5x fractograph) supported the conclusions that failure of the valve stem occurred by fatigue as a result of a combination of a nonuniform bending load, which caused a mild stress-concentration condition, and a high operating temperature in a corrosive environment. When the microstructure near the stem surface was examined, it was apparent that carbide spheroidization had occurred. Also, there was a coarsening of the carbide network within the austenite grains. The microstructure indicated that the underhead region of the valve was heated to about 930 deg C (1700 deg F) during operation. The cause of fatigue fracture, therefore, was a combination of non-uniform bending loads and overheating. No recommendations were made.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c0046991
EISBN: 978-1-62708-234-1
..., which resulted from heating during welding. Electron probe x-ray microanalysis showed the outside surface of the tube did not have the protective chromium oxide scale normally found on Incoloy 800. The inside surface of the tube had a thin chromium oxide protective scale. This evidence supported...
Abstract
The outlet-piping system of a steam-reformer unit failed by extensive cracking at four weld locations. The welded system consisted of Incoloy 800 (Fe-32Ni-21Cr-0.05C) pipe and fittings. The exterior surfaces of the system were insulated with rock wool that did not contain weatherproofing. On-site visual examination and magnetic testing indicated severe external corrosion of most of the piping. The system showed extensive cracking in weld HAZ. One specimen indicated that corrosion extended to a depth of 3.2 mm and cracks were seen at the edge of the cover bead and in the HAZ of the weld. Metallographic examination showed that cracking was intergranular and that adjacent grain boundaries had undergone deep intergranular attack. Examination at higher magnification revealed heavy carbide precipitation, primarily at grain boundaries, indicating that the alloy had been sensitized, which resulted from heating during welding. Electron probe x-ray microanalysis showed the outside surface of the tube did not have the protective chromium oxide scale normally found on Incoloy 800. The inside surface of the tube had a thin chromium oxide protective scale. This evidence supported the conclusions that the deep oxidation greatly decreased the strength of the weld HAZ and cracking followed.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c0046371
EISBN: 978-1-62708-234-1
... any stainless steel from the spacer. Other items for investigation were the nature of the bond between the galled spot and the inner cone and any evidence of overtempering or rehardening resulting from localized overheating. Analysis (visual inspection, electron probe x-ray microanalysis, microscopic...
Abstract
When a roller-bearing assembly was removed from an aircraft for inspection after a short time in service, several areas of apparent galling were noticed around the inside surface of the inner cone of the bearing. These areas were roughly circular spots of built-up metal. The bearing had not seized, and there was no evidence of heat discoloration in the galled areas. The inner cone, made of modified 4720 steel and carburized for wear resistance, rode on an AISI type 630 (17-4 PH) stainless steel spacer. Consequently, it was desirable to determine whether the galled spots contained any stainless steel from the spacer. Other items for investigation were the nature of the bond between the galled spot and the inner cone and any evidence of overtempering or rehardening resulting from localized overheating. Analysis (visual inspection, electron probe x-ray microanalysis, microscopic examination, and hardness testing) supported the conclusions that galling had been caused by a combination of local overload and abnormal vibration of mating parts of the roller-bearing assembly. No recommendations were made.
Image
in Galling Wear on a Steel Inner Cone of a Roller-Bearing Assembly
> ASM Failure Analysis Case Histories: Failure Modes and Mechanisms
Published: 01 June 2019
Fig. 1 Evidence of galling, or adhesive wear, on the inner surface of a carburized 4720 steel inner cone of a roller bearing. Galling was confirmed by the use of electron probe x-ray microanalysis.
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Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.homegoods.c0049838
EISBN: 978-1-62708-222-8
... correspond to specific intermetallic compounds that are found in the aluminum-iron phase diagram. X-ray microanalysis of reaction zone at the aluminum wire/steel screw interface shown in <xref rid="c0049838-f2" ref-type="fig">Fig. 2(a)</xref> Table 1 X-ray microanalysis of reaction zone...
Abstract
An electron probe microanalyzer was applied to the study of service failures (due to severe heating) of aluminum wire connections in residential electrical circuits. Perturbed regions in which the composition underwent a change during the failure were revealed by optical and scanning electron microscopy of the contacts. A sequence of iron-aluminum compositions that shift from the pure aluminum of the wire to the nearly pure iron of the screw was revealed by analyses of two distinct layers formed on the aluminum/iron region. The compositions were found to correspond to specific intermetallic compounds found in the aluminum-iron phase diagram. Similar compositional variations were noted at the aluminum/brass interface. It was concluded that the failure of the electrical junction due to extreme heating was related to the formation of intermetallic compounds at the current carrying interfaces. These intermetallics were established to have a high resistance causing significant resistive heating.
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.
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
... 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...
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.
Image
in Metallurgical Investigation of a Prematurely Failed Roller Bearing Used in the Support and Tilting System of a Steel Making Converter Used in an Integrated Steel Plant
> ASM Failure Analysis Case Histories: Steelmaking and Thermal Processing Equipment
Published: 01 June 2019
Fig. 9 Electron probe microanalysis (EPMA) scans of brittle alumina stringers observed in the failed converter bearing sample. (a) Backscattered electron (BSE) image; (b) O 2 X-ray map; (c) Al X-ray map. All, 600×
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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
... spectrometer and was the model for the first commercial systems (see the article “Electron Probe X-Ray Microanalysis” in Materials Characterization Volume 10 of ASM Handbook. These systems consisted of an x-ray detector and single-crystal diffractometers that moved synchronously around the sample...
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.
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
... • Newbury D.E. and Ritchie N.W.M. , Electron Probe X-Ray Microanalysis , Materials Characterization , Vol 10 , ASM Handbook , ASM International , 2019 , 10.31399/asm.hb.v10.a0006638 ...
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
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.steel.c9001645
EISBN: 978-1-62708-232-7
...× Fig. 8 Energy-dispersive spectrometric (EDS) analysis of inclusion observed at the crack site on the fracture surface of the failed converter bearing sample, showing Ca, Al, and Si X-ray peaks indicating the presence of silicate inclusion Electron Probe Microanalysis Electron probe...
Abstract
An extensive metallurgical investigation was carried out on samples of a failed roller bearing from the support and tilting system of a basic oxygen furnace converter used in the steel melting shop of an integrated steel plant. The converter bearing was fabricated from low-carbon, carburizing grade steel and had failed in service within a year of fitting to a repaired shaft. Microscopic observations of both the broken roller and inner-race samples revealed subsurface cracking and preponderance of brittle oxide and other macroinclusions. Electron probe microanalysis studies confirmed that the brittle oxides that formed stringers were alumina, and the other macroinclusions were complex silicates. Both the alumina and silicate inclusions were deleterious to contact-fatigue properties. Microstructurally, the carburized regions of the broken roller and of inner-race samples contained high-carbon tempered martensite. Microhardness measurements revealed that. Although the core hardness of the roller and the inner-race samples were similar, the surface hardness of the roller was approximately 8.5 HRC units harder than that of the inner-race. SEM observations of the roller fracture surface revealed striations indicative of fatigue, and EDS analyses corroborated a high incidence of silicate inclusions at crack sites. The study suggests that the failure of the bearing occurred because the hardness difference between the roller bearing and the inner-race surfaces resulted in wear of the inner-race. The wear led to shaft misalignment and play during service. The misalignment, coupled with the presence of inclusions, caused fatigue failure of the roller bearing.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.petrol.c9001247
EISBN: 978-1-62708-228-0
.... 6 Inside surface of sample 2 showing general attack and precipitation effects. Etched with 10% oxalic acid. 500 × The results of electron probe microanalysts of a section taken from the unmarked sample are illustrated in the form of electron and X-ray images in Fig. 7 . These results...
Abstract
Three samples from a ruptured 316 stainless steel tube were examined. The tube, 114 mm OD, wall thickness 8.00 mm, with 13 mm thick 321 stainless steel fins welded to the outer surface of the tube, was part of a heater through which sour gas, containing methane plus H2S and CO, passed at 1150 psig. The sour gas was heated to 600 deg F by burners playing on the outside of the tube burning “sweet” gas plus air. The inner and outer surfaces of all samples showed evidence of corrosive attack. Electron probe microanalysis showed the corrosion products contained sulfur with iron, together with nickel to a lesser extent. Local thinning, cavitation, and ductile deformation markings associated with the unmatched sample taken from the center of the fire showed the tube ruptured as a result of overheating. Overheating while the temperature recorder was off the chart caused severe loss of tube strength, resulting in ductile rupture. The minimum overheating temperature could be deduced at around 1200 deg F due to the presence of a eutectic observed metallographically within the surface corrosion products.
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 Lifshin E. , Scanning Electron Microscopy and X-ray Microanalysis , Plenum Press , New York , 1991 Operation Electron-Optical Column Development of SEM Technology Backscattered Electrons Signal Detection and Display Secondary Electrons Brittle Failures Typical Fracture...
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
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006769
EISBN: 978-1-62708-295-2
... electron signals for imaging, and the characteristic x-ray signal emitted from the sample for composition identification. Secondary Electrons Secondary electrons are low-energy electrons emitted from the sample as a result of coulombic interactions between the incident electrons from the beam...
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 Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006943
EISBN: 978-1-62708-395-9
... 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. atomic force...
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
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0006548
EISBN: 978-1-62708-180-1
... modulus or modulus of elasticity; energy E elastic or storage modulus E viscous or loss modulus EAC environmentally assisted cracking EBSP electron backscattered pattern ECT equicohesive temperature EDM electric discharge machining EDS energy dispersive spectroscopy EDX energy-dispersive x-ray (analysis...
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 Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.petrol.c9001603
EISBN: 978-1-62708-228-0
... of a crack with embedded inclusions. X-ray analysis confirmed the presence of Fe, Si, Ca, and O ( Fig. 3 ). Fig. 3 (a) SEI photomicrograph of an inclusion embedded within a crack and X-ray analysis of (b) Fe, (c) Si, (d) Ca, and (e) O Inclusion entrapment can occur during steelmaking, casting...
Abstract
The genesis of failure of 6.1 mm thick electric resistance welded API 5L X-46 pipes during pretesting at a pressure equivalent to 90% of specified minimum yield strength was investigated. Cracks were found to initiate on the outer surface of the pipes in the fusion zone and propagate along the through-thickness direction. The presence of extensive decarburization and formation of a soft ferrite band within the fusion zone may have contributed to the nucleation of the cracks. Crack propagation was aided by the presence of exogenous inclusions entrapped within the fusion zone. Analysis of these inclusions confirmed the presence of Fe, Si, Ca, and O, indicating slag entrapment to be the most probable culprit.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001357
EISBN: 978-1-62708-215-0
... of the analysis; spectrums obtained by Auger electron spectroscopy and X-ray photoelectron microscopy (XPS) are shown respectively in Fig. 9 and 10 . Results of electron spectroscopy at two different Table 1 Results of electron spectroscopy at two different Point Depth, nm Elements detected...
Abstract
Two 20 MW turbines suffered damage to second-stage blades prematurely. The alloy was determined to be a precipitation-hardening nickel-base superalloy comparable to Udimet 500, Udimet 710, or Rene 77. Typical protective coatings were not found. Test results further showed that the fuel used was not adequate to guarantee the operating life of the blades due to excess sulfur trioxide, carbon, and sodium in the combustion gases, which caused pitting. A molten salt environmental cracking mechanism was also a factor and was enhanced by the working stresses and by the presence of silicon, vanadium, lead, and zinc. A change of fuel was recommended.
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