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transmission electron microscopy
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Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.steel.c9001490
EISBN: 978-1-62708-232-7
..., transmission electron microscopy, optical microscopy, and x-ray microanalysis in conjunction with dimensional analysis, phase diagrams and thermodynamics considerations were employed to evaluate the various hypotheses. All evidence pointed to an oxide mass in the area where the hole developed, likely...
Abstract
A steel pot used as crucible in a magnesium alloy foundry developed a leak that resulted in a fire and caused extensive damage. Hypotheses as to the cause of the leak included a defect in the pot, overuse, overheating, and poor foundry practices. Scanning electron microscopy, transmission electron microscopy, optical microscopy, and x-ray microanalysis in conjunction with dimensional analysis, phase diagrams and thermodynamics considerations were employed to evaluate the various hypotheses. All evidence pointed to an oxide mass in the area where the hole developed, likely introduced during the steelmaking process.
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in Failure of a Thick-Wall Casing for a Steam Turbine by Cracking
> ASM Failure Analysis Case Histories: Power Generating Equipment
Published: 01 June 2019
electron microscopy fractographs of four locations on the fracture surface. 7500×. Intergranular modes of fracture are shown in (b) and (c); a transgranular mode, typical of corrosion fatigue, is shown in (d). The fractograph in (e) was taken in the region of crack arrest and indicates an intergranular
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Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.mech.c0091475
EISBN: 978-1-62708-225-9
... , and intergranular separation, as shown in the stereo pair of Fig. 3 , which is characteristic of hydrogen embrittlement of high-stress steels. Debris from the final reaction to which the part was exposed has resulted in artifacts on the transmission electron microscopy (TEM) replicas, but there appears...
Abstract
A type 431 stainless steel mushroom-head closure fractured in service at a hydrogen pressure of 3000 atm. Fracture occurred at room temperature after miscellaneous chemical service that included exposures to hydrogen at temperatures from ambient to 350 deg C (662 deg F). Investigation (visual inspection and 2400x/6600x TEM analysis) supported the conclusion that failure was caused by hydrogen embrittlement, not SCC as might have been suspected. No recommendations were made.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.process.c0045918
EISBN: 978-1-62708-235-8
... on selected-area diffraction is provided in the article “Analytical Transmission Electron Microscopy” in Volume 10 of ASM Handbook , formerly 9th Edition Metals Handbook ). The diffraction pattern obtained most closely matched the pattern for niobium tetrafluoride. Auger analyses were conducted...
Abstract
Cracks, with no other damage, were observed in a niobium alloy (Nb-106) part when it was pulled from several months of protective storage for assembly into a rocket nozzle. SEM views showed the cracks to be intergranular, with contaminant particles on a large number of the grain facets. EDX analysis showed they consisted of niobium and fluorine. Plastic replicas, prepared by standard TEM techniques, were analyzed with selected-area electron diffraction, showing a pattern match for niobium tetrafluoride. Auger analyses showed electron spectra containing peaks representing carbon, oxygen, nitrogen, fluorine, and chlorine. Investigation into the processing history of the part showed the tenacious oxide film formed by the affinity of niobium for oxygen - even when heat treated in a vacuum – was removed with a combination of strong acids: nitric, hydrochloric, hydrofluoric, and lactic, resulting in the contaminants found on the surface. Thus, residues of the cleaning acid on the part had caused SCC during storage, with the tensile stresses necessary to generate SCC assumed to have been residual stresses from the heat treatment. Recommendation was made that more stringent cleaning procedures to remove any trace of the cleaning acids be used.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c9001681
EISBN: 978-1-62708-234-1
...). To assist in this procedure, a microstructural analysis was made of the cast components. This involved optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). IN SEM and STEM, microchemical analyses were...
Abstract
A microstructural analysis has been made of a burner nozzle removed from service in a coal gasification plant. The nozzle was a casting of a Co-29wt%Cr-19wt%Fe alloy. Extensive hot corrosion had occurred on the surface. There was penetration along grain boundaries, and corrosion products in these regions were particularly rich in S, and also contained Al, Si, O, and Cl. The grain boundaries contained Cr-rich particles which were probably Cr23-C6 type carbides. In the matrix, corrosion occurred between the Widmanstatten plates. Particles were found between these plates, most of which were rich in Cr and O, and probably were Cr2-O3 oxides. Other matrix particles were found which were rich in Al, O, and S. The corrosion was related to these grain boundary and matrix particles, which either produced a Cr-depleted zone around them or were themselves attacked.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.aero.c0006448
EISBN: 978-1-62708-217-4
... ( Fig. 1f ). Metallographic examination showed that the pitting progressed in an intergranular corrosive pattern ( Fig. 1g ). The microstructure was acceptable for type 440C martensitic stainless steel. Electron optical examination of the fractures by transmission electron microscopy produced...
Abstract
Three wing flap hinge bearings were received by the laboratory for analysis. The bearings were fabricated from chromium-plated type 440C martensitic stainless steel. The intergranular fracture pattern seen in the electron fractographs, coupled with the corrosion pits observed on the inner diam of the bearings, strongly suggested that failure initiated by pitting and progressed by SCC or hydrogen embrittlement from the plating operation. It was recommended that the extent of the flap hinge bearing cracking problem be determined by using nondestructive inspection because it is possible to crack hardened type 440C during the chromium plating process. An inspection for pitting on the bearing inner diam was also recommended. It was suggested that electroless nickel be used as a coating for the entire bearing. A review of the chromium plating and baking sequence was recommended also to ensure that a source of hydrogen is not introduced during the plating operation.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.power.c0089663
EISBN: 978-1-62708-229-7
... from the casing, showing the fracture surface at right. A large porosity defect can be seen at the upper right corner, near the broken-open tapped hole. (b) to (e) Transmission electron microscopy fractographs of four locations on the fracture surface. 7500×. Intergranular modes of fracture are shown...
Abstract
A crack was discovered in a cast steel (ASTM A 356, grade 6) steam turbine casing during normal overhaul of the turbine. The mechanical properties of the casting all exceeded the requirements of the specification. When the fracture surface was examined visually, an internal-porosity defect was observed adjoining a tapped hole. A second, much larger cavity was also detected. Investigation (visual inspection and 7500x SEM fractographs) supported the conclusions that failure occurred through a zone of structural weakness that was caused by internal casting defects and a tapped hole. The combination of cyclic loading (thermal fatigue), an aggressive service environment (steam), and internal defects resulted in gradual crack propagation, which was, at times, intergranular-with or without corrosive attack-and, at other times, was transgranular.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006945
EISBN: 978-1-62708-395-9
...-styrene size-exclusion chromatography scanning electron microscope short ber reinforced polymer secondary ion mass spectroscopy styrene-maleic anhydride sheet molding compound Society of Plastics Engineers superplastic forming structural reaction injection molding scanning transmission electron...
Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001031
EISBN: 978-1-62708-214-3
... Specifications Performance of Other Parts in Same or Similar Service Specimen Selection Chemical Analysis/Identification Transmission Electron Microscopy (TEM) Microprobe Analysis Visual Examination of General Physical Features Testing Procedure and Results Surface Examination Optical...
Abstract
Pinhole defects were found in a main combustion chamber made from NARloy-Z after an unexpectedly short time in service. Analysis indicated that the throat section of the liner had been exposed to very severe environmental conditions of high temperature and high oxygen content, which caused ductility loss and grain-boundary separation. The excessive oxygen content in the liner was attributed to diffusion from an oxygen-rich environment that had resulted from nonuniform mixing of propellants. The internal oxygen embrittled the alloy and reduced its thermal conductivity, which resulted in a higher hot-gas wall temperature and associated degradation of mechanical properties.
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
... submerged arc welding SC carbon saturation SCC stress-corrosion cracking SCE standard calomel electrode SCF stress concentration factor SE secondary electrons SEM scanning electron microscopy; second- ary electron microscopy SFRP short fiber reinforced polymer compos- ite S-L short transverse-longitudinal...
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001838
EISBN: 978-1-62708-241-9
... , 2006 , p 461 – 471 . 10.31399/asm.hb.v14b.a0005135 Introduction Hypotheses about Potential Metallurgical Root Causes Materials Testing Results Chemical Composition Mechanical Properties Focussed Ion Beam (FIB)/Transmission Electron Microscopy (TEM) Electron Probe Microanalysis...
Abstract
Stainless steel pipe (273-mm OD x 8-mm wall thickness) used in the fabrication of large manifolds developed crack-like decohesions during a routine inductive bending procedure. The imperfections, which were found near the outside diameter, were around 3 mm in length oriented in the circumferential direction and penetrated nearly 2 mm into the pipe wall. The pipes were made of titanium-stabilized austenitic stainless steel X6CrNiMoTi17-12-2. Six hypotheses were considered during the investigation, which ultimately concluded that the failure was caused by liquation cracking due to overheating.
Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001125
EISBN: 978-1-62708-214-3
... Scanning Electron Microscopy/Fractography Testing Procedure and Results Surface Examination Macrofractography Corrosion Morphology Metallography Microstructural Analysis Discussion The aluminum connector failed by ductile fracture, which indicates mechanical overload rather than...
Abstract
An 1100 aluminum alloy connector of a high-tension aluminum conductor steel-reinforced (ACSR) transmission cable failed after more than 20 years in service, in a region of consider able industrial pollution. The steel core was spliced with a galvanized 1020 carbon steel sheath. Visual examination showed that the connector had undergone considerable plastic deformation and necking before fracture. The steel sheath was severely corroded, and the steel splice was pressed off-center in the axial direction inside the connector. Examination of the fracture surface and micro-structural analysis indicated that the failure was caused by mechanical overload, which occurred because of weakening of the steel support cable by corrosion inside the fitting. The corrosion was ascribed to defective assembly of the connector which allowed moisture penetration.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.chem.c0048840
EISBN: 978-1-62708-220-4
... higher than that in the adjacent base metal. Thin-foil transmission electron microscopy (TEM) was also used to demonstrate that high dislocation densities occurred in the vicinity of welded-over notches. The dislocations were bowed and pinned, an observation that is not exclusively associated with strain...
Abstract
A spherical carbon steel fixed-catalyst bed reactor, fabricated from French steel A42C-3S, approximately equivalent to ASTM A201 grade B, failed after 20 years of service while in a standby condition. The unit was found to contain primarily hydrogen at the time of failure. The vessel had a type 304 stainless steel shroud around the catalyst bed as protection against the overheating that was possible if the gas bypassed the bed through the refractory material. The failure was observed to have begun at the toe of the shroud-support ring weld. The ring was found to have a number of small cracks at the root of the weld. The cleavage mode of fracture was confirmed by SEM. The presence of extensive secondary cracking and twinning (Neumann bands) where the fracture followed the line of the shroud-support ring was revealed by metallography. It was revealed by refinery maintenance records that the ring had been removed for hydrotest and welded without any postweld heat treatment. The final cause of failure was concluded to be cracking that developed during the installation of the new shroud ring. Stress-relief heat treatments were recommended to be performed to reduce residual-stress levels after welding.
Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001077
EISBN: 978-1-62708-214-3
.../Identification Material Metallography Microstructural Analysis Testing Procedure and Results Nondestructive Evaluation Magnetic Particle Inspection Surface Examination Stereomicroscopic Scanning Electron Microscopy/Fractography Scanning electron microscopy (SEM) examination...
Abstract
The failure of a spiral bevel gear from the transmission of a helicopter was discovered when the transmission was removed after an in-flight incident. Two adjacent teeth from the carburized AISI 9310 steel gear were found to have undergone fatigue failure. Internal initiation occurred in a region depleted of chromium and nickel. This condition coincides with a microstructural inhomogeneity consisting of large, soft ferrite grains. Its origin was probably contamination of the solidifying ingot during the consumable vacuum arc remelting operation.
Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001124
EISBN: 978-1-62708-214-3
... Leading to Failure Pertinent Specifications Testing Procedure and Results Nondestructive Evaluation Liquid Penetrant Inspection Visual Examination of General Physical Features Surface Examination Scanning Electron Microscopy/Fractography Crack Origins/Paths Metallography...
Abstract
Several wires in aluminum conductor cables fractured within 5 to 8 years of, service in Alaskan tundra. The cables were comprised of 19-wire strands; the wires were aluminum alloy 6201-T81. Visual and metallographic examinations of the cold-upset pressure weld joints in the wires established that the fractures were caused by fatigue loading attributable to wind/thermal factors at the joints. The grain flow at the joints was transverse to the wire axis, rendering the notches of the joints sensitive to fatigue loading. An additional contributory factor was intergranular corrosion, which assisted fatigue crack initiation/propagation. The failure was attributed to the departure of conductor quality from the requirements of ASTM B 398 and B 399, which specify that “no joints shall be made during final drawing or in the finished wire” and that the joints should not be closer than 15 m (50 ft). The failed cable did not meet either criterion. It was recommended that the replacement cable be inspected for strict compliance to ASTM requirements.
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
... Electron Microscopy and X-Ray Microanalysis , Springer , 2019 , p 481 – 489 , https://link.springer.com › book › 978-1-4939-6676-9 11. Pendse D.R. and Chin A.K. , Cathodoluminescence and Transmission Cathodoluminescence , Encyclopedia of Materials: Science and Technology , 2nd ed...
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.power.c9001679
EISBN: 978-1-62708-229-7
... stage shown in Figure 12 . They are small, approximately 5 µm in diameter, and appear to be ferrite. Figure 13 , a longitudinal section from this same area, shows the presence of stringers (probably ferrite). Transmission electron microscopy (TEM) was employed to identify these artifacts. Particles...
Abstract
Several mercury diffusion pump stages in the Tritium Purification process at the Savannah River Site (SRS) have been removed from service for scheduled preventive maintenance. These stages have been examined to determine if failure has occurred. Evidence of fatigue around the flange portion of the pump has been seen. In addition, erosion and cavitation inside the throat of the venturi tube and corrosion on the other surface of the venturi tube has been observed. Several measures are being examined in an attempt to improve the performance of these pumps. These measures, as well as the noted observations, are described. Six stages [two machined (MP) and four electron beam (EB) welded] from the mercury diffusion pumps operating in the Tritium Purification process at SRS have been analyzed to determine their condition after nine months of usage. Several cracks were found around the necked region of the two MP stages. The EB welded stages, however, seemed to perform better in service; only two of four stages showed cracking. The cracking is caused by fatigue that has been enhanced by high stresses and tritium in the flange area. The EB welded stage appears to be a step in the right direction. Since the EB weld is a shrink fit, the surface is in compression, thereby eliminating crack propagation. In addition, shot peening has been employed to produce a compressive material surface since fatigue usually originates at the surface. Pitting was observed down the throat of the venturi. This pitting was caused by cavitation and erosion along the length of the venturi tube. Corrosion and pitting was seen on the exterior walls of the diffuser tubes. Stress-corrosion cracks were observed emanating from these corrosion pits. The corrosion likely occurred from the chloride ions present in the process cooling water. Shot peening is now being used in an attempt to place the outside of the diffuser tube in compression to eliminate the stress-corrosion cracking.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003527
EISBN: 978-1-62708-180-1
... or sectioning for scanning electron microscopy examination and/or metallography. It is important to photograph the component at each stage of the process to retain the visual information available and the component condition at each step. Field Photographic Documentation Composition Photographic...
Abstract
This article reviews photographic principles, namely, visual examination, field photographic documentation, and laboratory photographic documentation, as applied to failure analysis and the specific techniques employed in both the field and laboratory. It provides information on the photographic equipment used in failure analysis and on film and digital photography. The article describes the basics of photography and the uses of different types of lighting in photography of a fractured surface. The article also addresses the techniques involved in macrophotography and microscopic photography as well as other special techniques.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001293
EISBN: 978-1-62708-215-0
... at the machined radius within a region that was severely pitted. Electron microscopy revealed that most of the fracture surface failed in an intergranular fashion. Energy dispersive spectroscopy determined that deposits of sand, corrosion and salts were found within the pits. The failure started by hydrogen...
Abstract
A forged, cadmium-plated electroslag remelt (ESR) 4340 steel mixer pivot support of the rotor support assembly located on an Army attack helicopter was found to be broken in two pieces during an inspection. Visual inspection of the failed part revealed significant wear on surfaces that contacted the bushing and areas at the machined radius where the cadmium coating had been damaged, which allowed corrosion pitting to occur. Optical microscopy showed that the crack origin was located at the machined radius within a region that was severely pitted. Electron microscopy revealed that most of the fracture surface failed in an intergranular fashion. Energy dispersive spectroscopy determined that deposits of sand, corrosion and salts were found within the pits. The failure started by hydrogen charging as a result of corrosion, and was aggravated by the stress concentration effects of pitting at the radius and the high notch sensitivity of the material. The failure mechanism was hydrogen-assisted and was most likely a combination of stress-corrosion cracking and corrosion fatigue. Recommendations were to improve the inspection criteria of the component in service and the material used in fabrication.
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