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quantitative microscopy
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Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.power.c9001571
EISBN: 978-1-62708-229-7
... of three people hired to perform the review [ 7 ]. We concluded that the temperature estimates were reasonable and suggested that quantitative microscopy, aided by selective etching, might permit a more precise estimate of the degree of thermal exposure. Subsequently, the writer obtained the metallographic...
Abstract
The accident at Three Mile Island Unit No. 2 on 28 March 1979 was the worst nuclear accident in US history. By Jan 1990, it was possible to electrochemically machine coupons from the lower head using a specially designed tool. The specimens contained the ER308L stainless steel cladding and the A533 Grade B plate material to a depth of about mid-wall. The microstructures of these specimens were compared to that of specimens cut from the Midland, Michigan reactor vessel, made from the same grade and thickness but never placed in service. These specimens were subjected to known thermal treatments between 800 and 1100 deg C for periods of 1 to 100 min. Microstructural parameters in the control specimens and in those from TMI-2 were quantified. Selective etchants were used to better discriminate desired microstructural features, particularly in the cladding. This report is a progress report on the quantification of changes in both the degree of carbide precipitation and delta ferrite content and shape in the cladding as a function of temperature and time to refine the estimates of the maximum temperatures experienced.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.steel.c9001532
EISBN: 978-1-62708-232-7
... roll quality, viz. characteristics of graphite, carbides, martensite, etc., have been extensively studied through optical microscopy, quantitative image analysis (QIA), and electron-probe microanalysis (EPMA). These are discussed in the context of spalling propensity and roll life. Hardness Hot...
Abstract
Work rolls made of indefinite chill double-poured (ICDP) iron are commonly used in the finishing trains of hot-strip mills (HSMs). In actual service, spalling, apart from other surface degeneration modes, constitutes a major mechanism of premature roll failures. Although spalling can be a culmination of roll material quality and/or mill abuse, the microstructure of a broken roll can often unveil intrinsic inadequacies in roll material quality that possibly accentuate failure. This is particularly relevant in circumstances when rolls, despite operation under similar mill environment, exhibit variations in roll life. The paper provides an insight into the microstructural characteristics of spalled ICED HSM work rolls, which underwent failure under similar mill operating environment in an integrated steel plant under the Steel Authority of India Limited. Microstructural features influencing ICDP roll quality, viz. characteristics of graphite, carbides, martensite, etc., have been extensively studied through optical microscopy, quantitative image analysis (QIA), and electron-probe microanalysis (EPMA). These are discussed in the context of spalling propensity and roll life.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001787
EISBN: 978-1-62708-241-9
... in service. Samples of the failed bit were analyzed using optical and scanning electron microscopy, quantitative metallography, and chemical analysis. The composition was found to be that of 18CrNi3Mo steel. Investigators also found evidence of inclusions and prior austenite grain size, although...
Abstract
A masonry type drill bit, designed for impact drilling in rock, fractured after a short time in service. Samples of the failed bit were analyzed using optical and scanning electron microscopy, quantitative metallography, and chemical analysis. The composition was found to be that of 18CrNi3Mo steel. Investigators also found evidence of inclusions and prior austenite grain size, although it was determined that neither played a role in the failure. Rather, according to test data, the failure occurred because of stress concentration (due to geometric discontinuities along the tooth profiles) and the cumulative effect of torque and force loading (the byproduct of continuous twisting and axial impact). Cracks readily initiate under these conditions then propagate quickly through what was found to be networks of tempered martensite, thus resulting in premature failure.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003536
EISBN: 978-1-62708-180-1
.... , Vol 21A , 1990 , p 1201 – 1207 23. Underwood E.E. , Quantitative Stereology , Addison Wesley Publishing Co. , 1970 24. DeHoff R.T. and Rhines F.N. , Quantitative Microscopy , McGraw Hill Publishing Co. , New York , 1968 25. Baddeley A.J. , Gundersen...
Abstract
The quantitative characterization of fracture surface geometry, that is, quantitative fractography, can provide useful information regarding the microstructural features and failure mechanisms that govern material fracture. This article is devoted to the fractographic techniques that are based on fracture profilometry. This is followed by a section describing the methods based on scanning electron microscope fractography. The article also addresses procedures for three-dimensional fracture surface reconstruction. In each case, sufficient methodological details, governing equations, and practical examples are provided.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006759
EISBN: 978-1-62708-295-2
... be sampled to later perform chemical analysis using other methods. Electron microprobe analysis or electron probe microanalysis is an alternative to scanning electron microscopy for performing chemical analysis. Electron probe microanalysis in conjunction with WDS is considered more quantitative than...
Abstract
Chemical analysis is a critical part of any failure investigation. With the right planning and proper analytical equipment, a myriad of information can be obtained from a sample. This article presents a high-level introduction to techniques often used for chemical analysis during failure analysis. It describes the general considerations for bulk and microscale chemical analysis in failure analysis, the most effective techniques to use for organic or inorganic materials, and examples of using these techniques. The article discusses the processes involved in the chemical analysis of nonmetallics. Advances in chemical analysis methods for failure analysis are also covered.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001367
EISBN: 978-1-62708-215-0
... the inside, cooled in liquid nitrogen, and fractured open to enable analysis of a fracture surface. Standardless semi-quantitative scanning electron microscopy/energy-dispersive x-ray spectrometry (SEM/EDS) analysis revealed a high sodium content in the corrosion product ( Fig. 2 ). The base metal elements...
Abstract
Cracking was discovered in an in-service, second-stage turbine impeller during a downtime inspection. The fabricated 4300 series low-alloy steel impeller was used in a compressor in an industrial petrochemical plant. It was also reported that a process upset had allowed a 10% NaOH solution to be ingested by the unit. Routine magnetic particle inspection revealed numerous cracks in the hub area and vane tips of the second-stage impeller Additionally, the outside surface of the backing plate showed a cyclic pattern of cracks. An overview of a conventional, systematic metallurgical approach to failure analysis to confirm that the cracking was caused by a caustic stress-corrosion cracking mechanism is presented.
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
... for failure analysis, qualitative results are adequate, but the method can determine quantitative elemental compositions to a precision of 0.01 wt% with relative accuracies of ±5%, depending on the specific material, type of x-ray detector used, the method of data analysis employed, and, as always, the skill...
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.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 Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001365
EISBN: 978-1-62708-215-0
... removed from the impeller body. The maximum defect depth is about 2.5 mm (0.10 in.). Scanning Electron Microscopy/Fractography Several areas that appeared to have the most severe surface damage were sectioned from the impeller body and fractured open in the laboratory. These surfaces were...
Abstract
An investigation was conducted to determine the cause of numerous cracks and other defects on the surface of a cast ASTM A743 grade CA-15 stainless steel main boiler feed pump impeller. The surface was examined using a stereomicroscope, and macrofractography was conducted on several cross sections removed from the impeller body. Areas that appeared to have the most severe surface damage were sectioned, fractured open, and examined using SEM. The chemistry of the impeller and an apparent repair weld were also analyzed. The examination indicated that the cracks were shrinkage voids from the original casting process. Surface repair welds had been used to fill in or cover over larger shrinkage cavities. It was recommended that more stringent visual and nondestructive examination criteria be established for the castings.
Series: 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
...) before it was fractured open in the laboratory. Fig. 2 Secondary crack after it was fractured open in the laboratory. Testing Procedure and Results Surface Examination Scanning Electron Microscopy Fractography Both primary and secondary cracks were examined using a scanning...
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.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001281
EISBN: 978-1-62708-215-0
... segments. (a) Leading edges. (b) Trailing edges. Fig. 2 Representative leading (a) and trailing (b) edges of the nozzles. Testing Procedure and Results Surface Examination Scanning Electron Microscopy/Fractography Fig. 3 shows an area exhibiting missing coating. Examination...
Abstract
The first-stage nozzles of a high-pressure turbine section of an industrial gas turbine exhibited leading and trailing-edge deterioration. The nozzles were made of X-40, a cobalt-base alloy, and were aluminide coated. Failure analysis determined that the deterioration was the result of hot corrosion caused by a combination of contaminants, cooling-hole blockage, and coating loss.
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
... × 10 −9 A probe current using proprietary application software. Microprobe analysis was also performed on the polished samples in an EPMA to quantitatively determine the variation of carbon in the case and core regions, as well as to determine the types of NMI present. The EPMA studies were carried...
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
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001072
EISBN: 978-1-62708-214-3
... and the cover. Applications The impeller was from a multistage, centrifugal unit designed to carry moist air. The unit was operated in a chemical plant. Specimen Selection Because corrosion rendered the larger crack faces useless for scanning electron microscopy (SEM) with respect to fractography...
Abstract
Radial cracking occurred adjacent to 11 vanes in a 19-vane impeller operating in a chemical plant environment. The impeller vanes were fillet welded to both the disk and the cover Cracks were next to the fillet welds and near the cover outer diameter They generally did not extend to the outer diameter. The entire impeller surface was tested by the dry magnetic particle method. Visual and microstructural examinations revealed intergranular cracking. Energy-dispersive spectroscopy of corrosion products contained in the cracks disclosed the presence of chlorine and sulfur The failure was attributed to stress-corrosion cracking caused by a corrosive atmosphere.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.aero.c9001605
EISBN: 978-1-62708-217-4
... position, topology, and details of interactions with microstructural features. The aim of this investigation was to use quantitative fractography as a tool to extract information, including striation spacing and size of the stretched zone, in order to make a direct correlation with fracture mechanic...
Abstract
After a quick-release fitting of an ejection seat broke, an investigation was performed to determine the manner and cause of crack propagation. Most fractography-based investigations aim to characterize only qualitative characteristics, such as the fracture orientation and origin position, topology, and details of interactions with microstructural features. The aim of this investigation was to use quantitative fractography as a tool to extract information, including striation spacing and size of the stretched zone, in order to make a direct correlation with fracture mechanic concepts. As the crack propagated, striations were created on the fracture surface as a result of service-induced load changes. The size of the striations were measured to estimate crack propagation rate. Remaining lifetime estimates were also made. The dimensions of plastically stretched zones found at the tips of the cracks were evaluated using electron micrograph stereo image pairs to characterize local fracture toughness. To complete the failure analysis, nondestructive evaluation, metallographic examination, and chemical investigations were carried out. No secondary cracks could be found. Most of the broken parts showed that the microstructure, the hardness, and the chemical composition of the Al-alloy were within the specification, but some of the cracked parts were manufactured using a different material than that specified.
Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001120
EISBN: 978-1-62708-214-3
... with striations characteristic of fatigue. Chemical Analysis/Identification A quantitative chemical analysis was conducted on the segment. The composition is shown in Table 1 . Based on the chemical analysis, the die complied with the chemical requirements for ASTM A681-89 H13 tool steel (see Table 1...
Abstract
A segment from a premium-quality H13 tool steel die for die casting of aluminum failed after only 700 shots. The segment was subjected to visual, macroscopic, hardness, and metallographic testing. The investigation revealed that failure occurred as a result of fatigue at an electrical-discharge-machined surface where the resulting rehardened layer had not been removed. This rehardened layer had cracked, providing a source for fatigue initiation.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003532
EISBN: 978-1-62708-180-1
... polishing. The article also describes the microstructure examination of various materials, with emphasis on failure analysis, and concludes with information on the examination of replicas with light microscopy. References References 1. Vander Voort G.F. , Met. Eng. Q. , Vol 15 , May...
Abstract
This article provides a discussion on the metallographic techniques used for failure analysis, and on fracture examination in materials, with illustrations. It discusses various metallographic specimen preparation techniques, namely, sectioning, mounting, grinding, polishing, and electrolytic polishing. The article also describes the microstructure examination of various materials, with emphasis on failure analysis, and concludes with information on the examination of replicas with light microscopy.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001292
EISBN: 978-1-62708-215-0
... of the struts was recommended. Crack propagation Fractography Military planes Scanning electron microscopy 7049 UNS A97049 Fatigue fracture Background A crack was detected in one arm of the right-hand horizontal brace of the nose landing gear shock strut from a large military aircraft...
Abstract
A crack was detected in one arm of the right-hand horizontal brace of the nose landing gear shock strut from a large military aircraft. The shock strut was manufactured from a 7049 aluminum alloy forging in the shape of a delta. A laboratory investigation was conducted to determine the cause of failure. It was concluded that the arm failed because of the presence of an initial defect that led to the initiation of fatigue cracking. The fatigue cracking grew in service until the part failed by overload. The initial defect was probably caused during manufacture. Fleet-wide inspection of the struts was recommended.
Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001081
EISBN: 978-1-62708-214-3
..., the cracks were pried open ( Fig. 4 ). Scanning electron microscopy (SEM) of the bolt hole cracks clearly established that a low-cycle fatigue mechanism was responsible for initiating thumbnail ( Fig. 5 ) or corner-type ( Fig. 5 ) cracks. In most specimens, cracks initiated near the subsurface primary...
Abstract
Several compressor disks in military fighter and trainer aircraft gas turbine engines cracked prematurely in the bolt hole regions. The disks were made of precipitation-hardened AM355 martensitic stainless steel. Experimental and analytical work was performed on specimens from the fifth-stage compressor disk (judged to be the most crack-prone disk in the compressor) to determine the cause of the failures. Failure was attributed to high-strain low-cycle fatigue during service. It was also determined that the cyclic engine usage assumed in the original life calculations had been under estimated, which led to low-cycle fatigue cracking earlier than expected. Fracture mechanics analysis of the disks was carried out to assess their damage tolerance and to predict safe inspection intervals.
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 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
... tube sections from each end of one economizer tube. One of the tube sections had leaked adjacent to the weld at the header. The microstructure and elemental composition of the tube material were consistent with type 304 stainless steel in the annealed condition. Quantitative chemical analyses were...
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.
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