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metallographic sample preparation
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Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006757
EISBN: 978-1-62708-295-2
... the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed...
Abstract
Examination of a damaged component involves a chain of activities that, first and foremost, requires good observation and documentation. Following receipt and documentation, the features of damage can be recorded and their cause(s) investigated, as this article briefly describes, for typical types of damage experienced for metallic components. This article discusses the processes involved in visual or macroscopic examination of damaged material; the interpretation of fracture features, corrosion, and wear damage features; and the analysis of base material composition. It covers the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.process.c9001667
EISBN: 978-1-62708-235-8
... joints Ti-6Al-4V Joining-related failures Introduction The nondestructive analysis of materials performed on-site required specialized equipment, and the careful development of metallographic preparation procedures. These procedures should be designed to minimize the damage to the material...
Abstract
Nondestructive metallographic examination of materials frequently must be performed on-site when the component in question cannot be moved or destructively examined. Often, it is imperative that specific microstructural information (i.e., material type, heat treatment condition, homogeneity, etc.) be obtained either before initial use of a component, or before the use of a component can be safely resumed. In this paper, the use of standard metallurgical laboratory equipment, and the procedures required to conduct nondestructive on-site metallographic analyses of engineering materials, is presented. As an example, the materials and metallographic techniques employed in an actual on-site investigation of a gas tungsten-arc weldment joining two large diameter Ti-6Al-4V alloy cylinders are discussed in depth to illustrate what can be accomplished.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001277
EISBN: 978-1-62708-215-0
..., polishing, and etching. The prepared sections were examined using a metallographic microscope to assess microstructure and internal and external surface conditions. Copper deposits, voids, and microfissures beneath the deposits were observed along the internal surfaces of the tube samples. Metallic...
Abstract
Waterwall tube failure samples removed from a coal- and oil-fired boiler in service for 12 years exhibited localized underdeposit corrosion and hydrogen damage. EDS and XRD revealed that bulk internal deposits collected from the tubes contained metallic copper which can accelerate corrosion through galvanic effects and can promote hydrogen damage. Ultrasonic testing was recommended to locate tubes with severe gouging and corrosion, which are suspect locations for hydrogen damage. The source of the copper should be identified and future chemical cleaning of the boiler should address its presence in the waterwall tubes.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.aero.c0091318
EISBN: 978-1-62708-217-4
... containing 15 vol% concentrated nitric acid (HNO 3 ) and 3 vol% concentrated hydrofluoric acid (HF) to remove heat discoloration and scale and were then immersed in the three sodium hypochlorite solutions for several days. None of the samples showed any sign of corrosion. Metallographic Inspection...
Abstract
Two freshwater tanks (0.81 mm (0.032 in) thick, type 321 stainless steel) were removed from aircraft service because of leakage due to pitting and rusting on the bottoms of the tanks. One tank had been in service for 321 h, the other for 10 h. There had been departures from the specified procedure for chemical cleaning of the tanks in preparation for potable water storage. The sodium hypochlorite sterilizing solution used was three times the prescribed strength, and the process exposed the bottom of the tanks to hypochlorite solution that had collected near the outlet. Investigation (visual inspection, 95x unetched images, chemical testing with a 5% salt spray, chemical testing with sodium hypochlorite at three strength levels, samples were also pickled in an aqueous solution containing 15 vol% concentrated nitric acid (HNO3) and 3 vol% concentrated hydrofluoric acid (HF) and were then immersed in the three sodium hypochlorite solutions for several days) supported the conclusion that failure of the stainless steel tanks by chloride-induced pitting resulted from using an overly strong hypochlorite solution for sterilization and neglecting to rinse the tanks promptly afterward. Recommendations included revising directions for sterilization and rinsing.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c9001704
EISBN: 978-1-62708-218-1
... the welds contained a lighter-colored, uniform build-up of similar material. Samples of the deposits were removed for examination via energy dispersive spectroscopy (EDS). Following the collection of EDS samples, several corroded and one non-corroded weld sections were removed for metallographic examination...
Abstract
Several type 304 stainless steel fire truck water tanks developed through-wall leaks after being in service for approximately two years. One representative tank underwent a comprehensive laboratory analysis, which included metallographic examinations and chemical analyses. The examinations revealed a classic case of microbiologically influenced corrosion (MIC), which preferentially attacked the heat affected zones of the tank welds, resulting in the leaks.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.process.c0048751
EISBN: 978-1-62708-235-8
... to the weld seam, were revealed by metallographic examination (hot shortness). It was indicated by energy-dispersive spectroscopy that type 316 electrode was not used for the root pass and instead a nickel-copper alloy electrode was employed. It was thus concluded that cracking was caused due to the use...
Abstract
The presence of subsurface cracks in a longitudinal weld seam of an AISI type 316 stainless steel heat-exchanger shell was revealed by radiographic testing. Numerous intergranular cracks associated with the root pass of the weld, which had propagated both parallel and normal to the weld seam, were revealed by metallographic examination (hot shortness). It was indicated by energy-dispersive spectroscopy that type 316 electrode was not used for the root pass and instead a nickel-copper alloy electrode was employed. It was thus concluded that cracking was caused due to the use of an incorrect electrode for the root pass as these electrodes are crack sensitive if overheated. The weld seam was completely ground out and replaced with the correct electrode material as a corrective measure.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001391
EISBN: 978-1-62708-215-0
... through a sample from group 6 was metallographically prepared. It was reported that the sample exhibited a cracked solder fillet. Examination of the cross section revealed gross delamination of the terminations ( Fig. 9 ). So severe was the delamination that the encapsulant had flowed into the interface...
Abstract
Several surface-mount chip resistor assemblies failed during monthly thermal shock testing and in the field. The resistor exhibited a failure mode characterized by a rise in resistance out of tolerance for the system. Representative samples from each step in the manufacturing process were selected for analysis, along with additional samples representing the various resistor failures. Visual examination revealed two different types of termination failures: total delamination and partial delamination. Electron probe microanalysis confirmed that the fracture occurred at the end of the termination. Transverse sections from each of the groups were examined metallographically. Consistent interfacial separation was noted. Fourier transform infrared and EDS analyses were also performed. It was concluded that low wraparound termination strength of the resistors had caused unacceptable increases in the resistance values, resulting in circuit nonperformance at inappropriate times. The low termination strength was attributed to deficient chip design for the intended materials and manufacturing process and exacerbated by the presence of polymeric contamination at the termination interface.
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
..., 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...
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.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.power.c0048850
EISBN: 978-1-62708-229-7
.... Examination of the metallographic samples at higher magnification revealed that the microstructure of the failed pipe consisted of a matrix precipitate array, probably M 23 C 6 , and large σ-phase particles in the grain boundaries. Although void formation and propagation along the σ/austenite interface...
Abstract
Cracks on the outer surface near a hanger lug were revealed by visual inspection of a type 316 stainless steel main steam line of a major utility boiler system. Cracking was found to have initiated at the outside of the pipe wall or immediately beneath the surface. The microstructure of the failed pipe was found to consist of a matrix precipitate array (M23C6) and large s-phase particles in the grain boundaries. A portable grinding tool was used to prepare the surface and followed by swab etching. All material upstream of the boiler stop valve was revealed to have oriented the cracking normally or nearly so to the main hoop stress direction. Residual-stress measurements were made using a hole-drilling technique and strain gage rosettes. Large tensile axial residual stresses were measured at nearly every location investigated with a large residual hoop stress was found for locations before the stop valve. It was concluded using thermal stress analysis done using numerical methods and software identified as CREPLACYL that one or more severe thermal downshocks might cause the damage pattern that was found. The root cause of the failure was identified to be thermal fatigue, with associated creep relaxation.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001375
EISBN: 978-1-62708-215-0
... was taken from the fracture site to be examined for detrimental conditions capable of inducing or contributing to cracking. The samples were mounted and metallographically prepared and were examined in the unetched and etched conditions. The unetched structure in the sample taken from the fractured area...
Abstract
Three sprinkler system dry pipe valve castings (class 30 gray iron), two that had failed in service and one that had been rejected during machining because of porosity, were submitted for examination. The two failures consisted of cracks in a seating face. All three were from the same heat. Visual examination showed that the casting had cracked through a thin area in the casting sidewall. Evidence of a sharply machined corner at the fracture site was also discovered. Tensile testing and metallographic analysis revealed no metallurgical cause for the failure. It was recommended that the manufacturer work with the foundry to evaluate the criticality of core placement and to eliminate the undesired thin section.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006765
EISBN: 978-1-62708-295-2
... be performed with the scanning electron microscope (SEM) over the same magnification range as the LM, but examination with the latter is more efficient. This article describes the major operations in the preparation of metallographic specimens, namely sectioning, mounting, grinding, polishing, and etching...
Abstract
Metallographic examination is one of the most important procedures used by metallurgists in failure analysis. Typically, the light microscope (LM) is used to assess the nature of the material microstructure and its influence on the failure mechanism. Microstructural examination can be performed with the scanning electron microscope (SEM) over the same magnification range as the LM, but examination with the latter is more efficient. This article describes the major operations in the preparation of metallographic specimens, namely sectioning, mounting, grinding, polishing, and etching. The influence of microstructures on the failure of a material is discussed and examples of such work are given to illustrate the value of light microscopy. In addition, information on heat-treatment-related failures, fabrication-/machining-related failures, and service failures is provided, with examples created using light microscopy.
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
... 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...
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
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.chem.c9001655
EISBN: 978-1-62708-220-4
... and filled with nitric acid in preparation for service. Three weeks later the two acid tanks were found to be leaking from the bottom. Samples from the spent solvent tank revealed that pitting was located in a depressed area near a suction hole, beneath a black residue. It was concluded that the acid tanks...
Abstract
This investigation involved two AISI 304L acid storage tanks and one AISI 304L spent solvent tank from a sewage treatment facility. After installation, these tanks were hydrostatically tested using sewage effluent. No leaks were found and after a year or two, the tanks were drained and filled with nitric acid in preparation for service. Three weeks later the two acid tanks were found to be leaking from the bottom. Samples from the spent solvent tank revealed that pitting was located in a depressed area near a suction hole, beneath a black residue. It was concluded that the acid tanks failed by chloride-induced pitting initiated by microbial activity. Further, the spent solvent tank failed by a similar, but anaerobic mechanism. The use of the effluent for the hydrostatic test and the failure to remove it and clean and dry the tanks was the primary cause of failure. Localized carbide segregation in the original plate served as preferential corrosion sites. Had the tanks been hydrostatically tested in a proper manner, the pitting may not have occurred.
Series: 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
.... The samples were metallographically prepared according to ASTM E-3. Samples were mounted in a conductive mount to make use of the SEM for subsequent work. Mounted samples were sequentially sanded from 240–600 grit on silicon oxide paper. The samples were then sequentially polished using 3 and 0.3-micron...
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.
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
.../Identification Material and Weld Metallography Microstructural Analysis Sections were cut from the expansion joint and prepared for metallographic examination by grinding, polishing, and etching. The prepared sections were examined using a metallurgical microscope to assess microstructure...
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.c9001320
EISBN: 978-1-62708-215-0
... was prepared for metallographic examination. The typical morphology of the pitting is shown in Fig. 3 . The pits are elliptical and have an undercut morphology with subsurface extensions. This type of pitting is characteristic of acidic attack. Some pits were deposit-filled and appeared to be active. The most...
Abstract
Severe pitting was found on the internal surfaces of SA-210 Grade C waterwall tubing of a coal-fired boiler at a cogeneration facility. Metallographic examination showed the pits to be elliptical, having an undercut morphology with supersurface extensions,. a type of pitting characteristic of acidic attack. Energy-dispersive X-ray spectroscope revealed the presence of chlorine in the pit deposits, indicating that the pitting was promoted by underdeposit chloride attack. The presence of copper in deposits on the internal surface of the tubing may have acted as a secondary factor. Acidic conditions may have formed during a low-pH excursion that reportedly occurred several years prior. To prevent future failures, severely damaged tubing must be replaced. Internal deposit buildup must be removed by chemical cleaning to prevent further pitting. Water quality needs continued monitoring and maintenance to ensure that another low-pH excursion does not occur.
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
... etched with the chemical listed in Table 1 . Chemicals used in preparing metallographic samples. Table 1 Chemicals used in preparing metallographic samples. Metallographic etchant used for optical and scanning electron microscopy samples. 100 ml HCl + 5 ml 30% H 2 O 2 swab 1—5 sec, 25°C...
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.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.rail.c9001607
EISBN: 978-1-62708-231-0
... equiaxed dimpled rupture Metallographic Examination Longitudinal sections of the failed wires from the wire rope were prepared for metallographic examination. In the unetched condition, the samples showed a large population of silicates and oxides and a few nitrides and sulfides ( Fig. 6...
Abstract
Wire ropes, pulleys, counterweights, and connecting systems are used for auto tensioning of contact wires of electric railways. A wire rope in one such auto tensioning system suffered premature failure. Failure investigation revealed fatigue cracks initiating at nonmetallic inclusions near the surface of individual wire strands in the rope. The inclusions were identified as Al-Ca-Ti silicates in a large number of stringers, and some oxide and nitride inclusions were also found. The wire used in the rope did not conform to the composition specified for AISI 316 grade steel, nor did it satisfy the minimum tensile strength requirements. Failure of the wire rope was found to be due to fatigue; however, the ultimate fracture of the rope was the result of overload that occurred after fatigue failure had reduced the number of wire strands supporting the load.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001279
EISBN: 978-1-62708-215-0
... the rupture and one on either side of the rupture, remote from the failed area. An additional ring section was removed from Tube 4 remote from the damaged area. The ring sections were prepared for metallographic examination by grinding, polishing, and etching. The prepared sections were examined using...
Abstract
Tube 3 from a utility boiler in service for 13 years under operating conditions of 540 deg C (1005 deg F), 13.7 MPa (1990 psi) and 1,189,320 kg/h (2,662,000 lb/h) incurred a longitudinal rupture near its 90 deg bend while Tube 4 from the same boiler exhibited deformation near its bend. Metallographic examination revealed creep voids near the rupture in addition to graphite nodules. Exposure of the SA209 Grade T1A steel tubing to a calculated mean operating temperature of 530 deg C (983 deg F) for the 13 years resulted in graphitization and subsequent creep failure in Tube 3. The deformation in Tube 4 was likely the result of steam washing from the Tube 3 failure. Graphitization observed remote from the rupture in Tube 3 and in Tube 4 indicated that adjacent tubing also was susceptible to creep failure. In-situ metallography identified other graphitized tubes to be replaced during a scheduled outage.
Series: 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
... Chemical Analysis/Identification Material Metallographic Examination Microstructural Analysis Examination of metallographically prepared cross sections of the spool piece revealed microstructures of normalized low-carbon steel—namely, pearlite and ferrite. The cracks were intergranular...
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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