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SEM/EDS fracture surface analysis
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Book Chapter
Boiler Stack Economizer Tube Failure
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001825
EISBN: 978-1-62708-241-9
... longitudinal and transverse cracks SEM/EDS fracture surface analysis tensile stress 304 (austenitic wrought stainless steel) UNS S30400 Introduction This paper details the investigation of the failure of a tube from a boiler stack economizer. The economizer was in a boiler at an ethanol plant...
Abstract
A type 304 stainless steel tube that failed in a boiler stack economizer was analyzed to determine the cause. The investigation consisted of visual, SEM/EDS, and metallographic analysis. Several degradation mechanisms appeared to be at work, including pitting corrosion, chloride stress corrosion cracking, and fatigue fracture. Investigators concluded that the primary failure mechanism was fatigue fracture, although either of the other mechanisms may have eventually caused the tube to fail in the absence of fatigue.
Book Chapter
Fatigue Failure of a Circulating Water Pump Shaft
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001371
EISBN: 978-1-62708-215-0
.../Fractography The fracture initiation sites in samples A and B were examined in the SEM and subjected to EDS analysis in the as-received condition. Figures 3 show that the fracture surface in the initiation area had an intergranular morphology and was covered by a corrosion product. EDS analysis...
Abstract
A type 410 stainless steel circulating water pump shaft used in a fossil power steam generation plant failed after more than 7 years of service. Visual examination showed the fracture surface to be coated with a thick, spalling, rust-colored scale, along with evidence of pitting. Samples for SEM fractography, EDS analysis, and metallography were taken at the crack initiation site. Hardness testing produced a value of approximately 27 HRC. The examinations clearly established that the shaft failed by fatigue. The fatigue crack originated at a localized region on the outside surface where pitting and intergranular cracking had occurred. The localized nature of the initial damage indicated that a corrosive medium had concentrated on the surface, probably due to a leaky seal. Reduction of hardness to 22 HRC or lower and inspection of seals were recommended to prevent future failures.
Book Chapter
Liquid Metal Embrittlement of Bronze Rupture Discs
Available to PurchaseSeries: 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
... 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...
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
Failure of Tension Springs During Installation
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.mech.c0090994
EISBN: 978-1-62708-225-9
... strength range was 1689 to 1793 MPa (245 to 260 ksi). The finished springs were to be shot peened for greater fatigue resistance. Investigation (visual inspection, 3x images, 2% nital etched 148x SEM images, chemical analysis, hardness testing, and EDS analysis) supported the conclusion that the springs...
Abstract
Two large tension springs fractured during installation. The springs were manufactured from a grade 9254 chromium-silicon steel spring wire. The associated material specification allows wire in the cold-drawn or oil-tempered (quenched-and-tempered) condition. The specified wire tensile strength range was 1689 to 1793 MPa (245 to 260 ksi). The finished springs were to be shot peened for greater fatigue resistance. Investigation (visual inspection, 3x images, 2% nital etched 148x SEM images, chemical analysis, hardness testing, and EDS analysis) supported the conclusion that the springs failed during installation due to the presence of preexisting defects. Crack surfaces were found to be corroded and phosphate coated, indicating that the cracks occurred during manufacture. Installation, which presumably entailed some axial extension, resulted in ductile overload failure at the crack sites. Recommendations included evaluating the manufacturing steps to identify the process(es) wherein the cracking was likely occurring. It was further recommended that a suitable nondestructive method such as magnetic particle inspection be implemented.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.conag.c9001633
EISBN: 978-1-62708-221-1
... Abstract Failure analysis of a mobile harbor crane wheel hub that included SEM and EDS analyses demonstrated that the mechanism of failure was fatigue. The wheel hub was a ductile cast iron component that had been subjected to cyclic loading during a ten-year service period. The fracture...
Abstract
Failure analysis of a mobile harbor crane wheel hub that included SEM and EDS analyses demonstrated that the mechanism of failure was fatigue. The wheel hub was a ductile cast iron component that had been subjected to cyclic loading during a ten-year service period. The fracture surface of the fatigue failure also contained corrosion deposit, suggesting that cracking occurred over a period of time sufficient to allow corrosion of the cracked surfaces. Replacement and alignment of the failed wheel hub was recommended along with inspection of the nonfailed wheel hubs that remained on the crane.
Book Chapter
Failure Analysis of a Fractured Wrench Socket
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001784
EISBN: 978-1-62708-241-9
... Original A Original B Hardness (HRB) 16 (±1) 18 (±0.25) 15 (±0.9) Scanning Electron Microscopy (SEM)/Energy Dispersive Spectroscopy (EDS) Analysis Figure 4 shows scanning electron micrograph of the fractured wrench socket indicating two pure brittle outer layer with a core region...
Abstract
A 13/16-in. hex socket failed while in use. Analysis (hardness testing, optical and scanning electron microscopy, and EDS) revealed that the socket was made of low carbon steel formed in a powder metallurgy process. A number of flaws were found including nonuniform wall thickness, poor geometric design with sharp corners as stress raisers, and incomplete sintering evidenced by unsintered particles. These were determined to be the primary cause of failure, although inclusions on the fracture surface containing S and Al may have played a role as well.
Book Chapter
Caustic-Induced Stress-Corrosion Cracking of a Flue Gas Expansion Joint
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001324
EISBN: 978-1-62708-215-0
... electron microscope (SEM) to document fracture features. The fracture surface deposits were analyzed by energy dispersive x-ray spectoscopy (EDS). Figure 3 shows typical SEM photographs of the crack surfaces. The primary, secondary, and lab fracture surfaces exhibited the same fracture features. Fig...
Abstract
A type 430Ti stainless steel flue gas expansion joint cracked because of caustic-induced stress-corrosion cracking. Energy-dispersive X-ray spectroscope analysis of the fracture surface deposits revealed the presence of sodium and potassium—caustics in hydroxide form. Primary fracture surfaces were all similar in appearance, and a primary crack origin could not be identified. A secondary crack brought to fracture in the laboratory showed brittle, cleavage features rather than classic, tensile overload features. This suggested that the material was embrittled.
Book Chapter
Liquid Metal Embrittlement of Flange Connector Studs in Contact With Cadmium
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001102
EISBN: 978-1-62708-214-3
... embrittlement (LME). Fig. 6 SEM micrograph of a fracture surface, depicting a melted and resolidified cadmium layer over an intergranular topography. EDS analysis was performed at “A” (see Fig. 7 ). 1540×. Fig. 7 Cracks in stud 3, filled with cadmium. EDS analyses were performed at “B...
Abstract
Four cadmium-plated ASTM A193 grade B studs from a steam line connector associated with a power turbine failed unexpectedly in a nil-ductility manner. Fracture surfaces were covered with a light-colored, lustrous deposit. Optical microscope, SEM, and EDS analyses were conducted on sections from one of the studs and revealed that the coating on the fracture surface was cadmium. The fracture had multiple origins, and secondary cracks also contained cadmium. The fracture topography was intergranular. The failures were attributed to liquid metal embrittlement caused by the presence of a cadmium plating and operating temperatures at approximately the melting point of cadmium. It was recommended that components exposed to the cadmium be replaced.
Book Chapter
Fatigue Failure of Six Cap Screws From a Hydraulic Coupling
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001098
EISBN: 978-1-62708-214-3
... NR Molybdenum 0.20 NR Iron bal bal (a) NR, no requirement During the initial SEM examination, deposits on the fracture surfaces of screws No. 1 and 4 were examined in situ using energy-dispersive X-ray spectroscopy (EDS). EDS provides qualitative elemental analysis...
Abstract
Six ASTM A-574 steel cap screws from a hydraulic coupling failed after 3 months in service. The screws were replacements for smaller-diameter cap screws that had been installed during an outage. Six new cap screws were examined along with the failed screws. Eight fracture locations were identified—three at the head-to-shank fillet, four at the eighth thread root from the cap, and one at the sixth thread root from the cap. Fracture surfaces were examined using a stereomicroscope and SEM, and the fracture mode was shown to be transgranular. EDS on the fracture surfaces showed sulfur and chlorine in the surface deposits. The observations indicated that the screws had failed by fatigue. Insufficient preloading was considered to be the most likely cause of the fatigue cracking. It was recommended that the proper preload on the screws be verified and maintained.
Book Chapter
Damage of a Screw in the Seal Coupling
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.mech.c9001614
EISBN: 978-1-62708-225-9
... of the failed screw with fracture surface. SEM, 10× These so-called microfractographic fracture surface elements are specific to the method, or rather mechanism, of fracture. 4 Using these elements, it is possible to deduce the initial loading conditions of the mechanical part, as well as the role...
Abstract
The damage to a screw on the head of a 1.8 liter personal car engine was nucleated as the result of common disadvantageous environmental influences and reversed loads leading to corrosion fatigue.
Book Chapter
Surface Examination and Analysis of Plastics
Available to PurchaseSeries: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006943
EISBN: 978-1-62708-395-9
.... Scanning electron microscopy instruments combined with an energy-dispersive spectroscopy (EDS) attachment (also referred to as EDX) allow the elemental chemical analysis of plastic materials. The EDS analysis with an SEM instrument can produce additional information for the plastic surfaces. The SEM...
Abstract
This article discusses the operating principles, advantages, and limitations of scanning electron microscopy, atomic force microscopy, x-ray photoelectron spectroscopy, and secondary ion mass spectroscopy that are used to analyze the surface chemistry of plastics.
Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001088
EISBN: 978-1-62708-214-3
... fracture surface from specimen A was removed for analysis to determine material composition. Standardless, semiquantitative SEM/EDS element analyses of the fracture surface revealed a carbon steel shaft and a type 300 stainless steel weld nugget ( Fig. 4 and 5 ). Fig. 4 Standardless...
Abstract
A 25 mm (1 in.) diam carrier shaft failed suddenly during operation. The shaft failed near the toe of the 4.8 mm (316 in.) frame-to-shaft 60 deg and 120 deg submerged metal arc (SMA) tack welds after an unknown time in service. Material specifications called for the shaft to be made from SAE 1018 cold-rolled carbon steel. Carrier assembly components were made from type 300 stainless steel, and all nuts, spacers, and washers were to be SMA tack welded to the stainless steel frame. Chemical analyses (OES, SEM/EDS) showed the shaft to actually be made from SAE 1050 high-carbon steel and that a low-carbon steel welding procedure had been used. This resulted in incipient cracks in the stainless steel weld metal near the toes of the component-to-shaft welds. The hardnesses of the heat-affected zones were as high as 58 HRC, and they were grain coarsened. The parting of the shaft was determined to have been caused by an impact failure mechanism, with the origin at the incipient cracks in the weld metal. Additionally, the coarsened heat-affected zones were found to be hydrogen embrittled. The primary cause of the failure was the use of an unspecified material.
Book Chapter
Hydrogen Embrittlement Failure of Socket Head Cap Screws
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001101
EISBN: 978-1-62708-214-3
... and laboratory-opened fracture surfaces of the screw were examined with a stereomicroscope at magnifications of 7 to 45× and with a scanning electron microscope (SEM) at much higher magnifications. The fracture surfaces displayed similar fracture modes. Figure 2 shows the overall fracture surface. Figure 3...
Abstract
Several cadmium-plated carbon steel socket head cap screws that were part of a slide valve assembly on a regenerator line in a petrochemical plant failed during initial loading. Metallographic and XDS chemical analysis in conjunction with SEM examination of one failed and one unfailed cap screw indicated that the screws had failed by hydrogen embrittlement. The plating process was the likely source of the hydrogen. It was recommended that the remainder of the cap screws from the same lot as the failed screws be baked at approximately 190 deg C (375 deg F) for 24 h.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001801
EISBN: 978-1-62708-241-9
... arrows Semi-quantitative chemical analysis was performed using SEM/EDS and the results were listed in Table 1 . The data showed that rod “B” had low aluminum and that iron was present, which might be a surface contaminant. Rod “A” chemical analysis met the chemistry specification for ASTM F136...
Abstract
Both rods in a Harrington rod cervical stent failed after a short time in service. Metallurgical analysis revealed a significant number of notches as well as enlarged grain size in one of the two rods, rough shallow-cracked surfaces along the bend profiles, possible signs of corrosion, and fractures (on both rods) near indentations imparted by retaining clamps. The observations suggest that surface roughness and bending defects initiated cracking that led to the fatigue failure of the compromised rod, followed some time later by the overload fracture of the second rod.
Book Chapter
Ultrasonic Cleaning-Induced Failures in Medical Devices
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001841
EISBN: 978-1-62708-241-9
... testing. SEM analysis showed that striations were present on the fracture surface, indicating that a fatigue crack preceded the overload fracture as shown in Fig. 6 and 7 . Several other cracks were observed at multiple locations along the stent, shown in Fig. 8 . Fig. 6 SEM image of fractured...
Abstract
Ultrasonic cleaning is widely used in the production of medical devices such as guide wires and vascular implants. There are many cases, however, where cleaning frequencies have been close to the natural frequency of the device, producing resonant vibrations large enough to cause damage or premature failure. Several cases of ultrasonic cleaning-induced fatigue and corresponding failures of medical devices are examined in this review. Preventative measures to ensure that ultrasonic cleaning frequencies do not pose a threat are also provided.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001805
EISBN: 978-1-62708-241-9
... and 14 ; consistent with brittle fracture in steels. EDS analysis (not shown) revealed that the plating on the caster was zinc. Fig. 12 Stereomicroscope image of the fracture surface Fig. 13 SEM image of the fracture surface near the origin showing brittle cleavage Fig. 14 SEM...
Abstract
Several surgical tool failures were analyzed to understand why they occur and how to prevent them. The study included drills, catheters, and needles subjected to the rigors of biomedical applications such as corrosive environments, high stresses, sterilization, and improper cleaning procedures. Given the extreme conditions to which surgical tools can be exposed, and the potential for misuse, failures are inevitable and systematic methods for analyzing them are necessary to keep them in check.
Book Chapter
Failure Analysis of a Cracked Low-Pressure Turbine Blade
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001355
EISBN: 978-1-62708-215-0
... Microscopy Fractography Examination of the fracture surface in the SEM revealed a flat oxidized fracture, typical of fatigue. Pits were found at each of the three fracture origins. Two origins are shown in Fig. 3 . The pits were 0.013 to 0.076 mm (0.0005 to 0.003 in.) deep. On the machined surface...
Abstract
A cracked, martensitic stainless steel, low-pressure turbine blade from a 623 MW turbine generator was found to exhibit fatigue cracks during a routine turbine inspection. The blade was cracked at the first notch of the fir tree and the cracks initiated at pits induced by chloride attack. Examination of the blade microstructure at the fracture origins revealed oxide-filled pits and transgranular cracks. The oxide filled cracks appeared to have originated at small surface pits and probably propagated in a fatigue or corrosion-fatigue fracture mode. It was recommended that the sources of the chlorides be eliminated and that the remaining blades be inspected at regular maintenance intervals for evidence of cracking.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001333
EISBN: 978-1-62708-215-0
... electron microscope (SEM), and the inner and outer surface oxides/deposits were analyzed using EDS. In the SEM, the thick oxide/deposit on the inner surface near the fracture surface appeared to contain many constituents ( Fig. 9 ). These areas, as well as the oxide/deposit on the outer surface, were each...
Abstract
A low-carbon steel (St35.8) tube in a phthalic anhydride reactor system failed. Visual and stereomicroscopic examination of fracture surfaces revealed heavy oxide/deposits on the outer surface of the tube, tube wall thinning in the area of the fracture, and discolorations and oxides/deposits on the inner surface. Cross sections from the fracture surface were metallographically examined, and the deposits were analyzed. It was determined that the tube had thinned from the inner surface because of a localized overheating condition (probably resulting from a runaway chemical reaction within the tube) and then fractured, which allowed molten salt to flow into the tube.
Book Chapter
Metallographic Characterization of Liquid Metal Embrittlement in a Failed Locomotive Axle
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.rail.c9001719
EISBN: 978-1-62708-231-0
... electron image. The image revealed an intergranular mode of fracture as shown in Figures 12 , 13 . Next an energy dispersive scan (EDS) was taken of the surface to determine if copper penetration had occurred and wetted the surface. Fig. 12 SEM image of intergranular fracture surface from secondary...
Abstract
Metallography is an important component of failure analysis. In the case of a liquid metal embrittlement (LME) failure it is usually conclusive if a third phase constituent can be formed inside of the cracks after failure. In the case where it is necessary to characterize the third phase material, one can use various x-ray spectrographic techniques in conjunction with a scanning electron microscope (SEM). This study describes those metallographic and SEM analysis techniques for determining the mode of failure for a locomotive traction motor by LME.
Book Chapter
Stress-Corrosion Cracking of a Teflon-Lined Steel Pipe in Sulfuric Acid Service
Available to PurchaseSeries: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001066
EISBN: 978-1-62708-214-3
... Material Qualitative chemical analysis of the spool piece material was performed using SEM and energy-dispersive X-ray spectroscopy (EDS). Results indicated that the alloy composition was consistent with low-carbon steel. Coatings or Surface Layers SEM/EDS analysis of the fracture surfaces...
Abstract
A flanged 100 mm (4 in.) diam low-carbon steel spool piece lined with Teflon was removed from a sulfuric acid denitrification system after cracks were observed in the painted coating. Visual and microstructural examination along with SEM fractography revealed scaled iron oxides on all opened crack surfaces. The surfaces had a faceted morphology, indicating intergranular fracture. Cracks originated at the interface between the tube and the Teflon liner Corrosion products were found caked into the intergranular region between the liner and the spool. The portion of the liner that had been exposed to the process stream was discolored. Failure of the spool was attributed to stress-corrosion cracking promoted by the presence of nitrates. Nitric acid contaminant in the sulfuric acid stream had diffused through the liner and accumulated in the annular space. Use of a liner that is more impermeable to the diffusion of ionic species was recommended.
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