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Epoxy
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Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001798
EISBN: 978-1-62708-241-9
... Carbon and oxygen contents of epoxy resin encapsulants Table 2 Carbon and oxygen contents of epoxy resin encapsulants Specimen C (wt.%) O (wt.%) C/O Normal 71.97 28.03 2.57 Softened 70.52 29.48 2.39 Fluid 70.27 29.73 2.36 Typical parameters in three TGA curves...
Abstract
The crosslinked epoxy resin encapsulant protecting an electromagnetic valve coil failed during long-term storage and was examined to determine the cause. The investigation included fault-tree analysis, FTIR and EDX spectroscopy, and differential scanning calorimetry with thermogravimetric analysis. Based on test data, the epoxy resin had not been properly cured and was hydrolyzed in its compromised state because of humidity. Hence, the depolymerized material gradually softened to the point where the effect of creep caused it to flow, ultimately causing the failure.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c0048498
EISBN: 978-1-62708-234-1
... Abstract A graphite-epoxy tapered-box structure, which consisted of two honeycomb skin panels fastened to a spanwise spar with intermediate chordwise ribs, fractured during testing. Hinge-line deflection of the front spar was revealed. Through-thickness cracks in the forward and trailing edges...
Abstract
A graphite-epoxy tapered-box structure, which consisted of two honeycomb skin panels fastened to a spanwise spar with intermediate chordwise ribs, fractured during testing. Hinge-line deflection of the front spar was revealed. Through-thickness cracks in the forward and trailing edges of the compression-loading skin panel were revealed by nondestructive visual examination. A band of de-lamination between the areas of through-thickness skin fracture at the front and rear spar was revealed. A map of the local directions of crack propagation over the fracture surface was generated by the orientation of river patterns and resin microflow during microscopic examination of sectioned samples of the panel. It was discovered that crack initiation occurred at the periphery of a fastener hole located at the front spar. Propagation occurred chordwise across the compression-loaded skin panel. As a corrective measure, the fastener spacing was reduced to prevent the buckling mode that precipitated fracture.
Image
in Hydrogen Embrittlement of Aircraft Components
> ASM Failure Analysis Case Histories: Air and Spacecraft
Published: 01 June 2019
Fig. 3 Corrosion pitting and cracking appeared under the green (G) epoxy primer and gray paint (P) near the start of fracture of Fig. 2 . Magnification 420 times.
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in Failure Analysis of Epoxy Resin Encapsulant During a Long-Term Storage
> Handbook of Case Histories in Failure Analysis
Published: 01 December 2019
Fig. 1 Curing mechanism of epoxy resin with anhydride as curing agent
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in Failure Analysis of Epoxy Resin Encapsulant During a Long-Term Storage
> Handbook of Case Histories in Failure Analysis
Published: 01 December 2019
Fig. 2 Fault tree for failure of epoxy resin encapsulant
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in Failure Analysis of Epoxy Resin Encapsulant During a Long-Term Storage
> Handbook of Case Histories in Failure Analysis
Published: 01 December 2019
Fig. 3 FTIR spectra of epoxy resin encapsulants ( a ) The whole spectra ( b ) Magnified spectra of carbonyl group
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in Failure Analysis of Epoxy Resin Encapsulant During a Long-Term Storage
> Handbook of Case Histories in Failure Analysis
Published: 01 December 2019
Fig. 4 EDS spectra of epoxy resin encapsulants
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in Failure Analysis of Epoxy Resin Encapsulant During a Long-Term Storage
> Handbook of Case Histories in Failure Analysis
Published: 01 December 2019
Fig. 5 TGA curves of epoxy resin encapsulants
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in Failure Analysis of Epoxy Resin Encapsulant During a Long-Term Storage
> Handbook of Case Histories in Failure Analysis
Published: 01 December 2019
Fig. 6 DSC curves of epoxy resin encapsulants
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Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.process.c0045926
EISBN: 978-1-62708-235-8
... Abstract A batch of bimetal foil/epoxy laminates was rejected because of poor peel strength. The laminates were manufactured by sintering a nickel/phosphorus powder layer to a copper foil, cleaning, then chromate conversion coating the nickel-phosphorus surface, and laminating the nickel...
Abstract
A batch of bimetal foil/epoxy laminates was rejected because of poor peel strength. The laminates were manufactured by sintering a nickel/phosphorus powder layer to a copper foil, cleaning, then chromate conversion coating the nickel-phosphorus surface, and laminating the nickel-phosphorus side of the clad bimetal onto an epoxy film, so that the end product contained nickel-phosphorus sandwiched between copper and epoxy, with a chromate conversion layer on the epoxy side of the nickel-phosphorus. Peel testing showed abnormally low adhesion strength for the bad batch of peel test samples. Comparison with normal-strength samples using XPS indicated an 8.8% Na concentration on the surface of the bad sample; the good example contained less than 1% Na on the surface. After 15 min of argon ion etching, depth profiling showed high concentrations of sodium were still evident, indicating that the sodium was present before the chromate conversion treatment was performed. A review of the manufacturing procedures showed that sodium hydroxide was used as a cleaning agent before the chromate conversion coating. Failure cause was that apparently the sodium hydroxide had not been properly removed during water rinsing. Thus, recommendation was to modify that stage in the processing.
Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001059
EISBN: 978-1-62708-214-3
... atmosphere and concentrating under the insulation around the support rings. A complete insulation evaluation, including repair or replacement, was recommended to prevent chloride buildup. Painting of the steel surface with an epoxy-phenolic or epoxy-coal tar was also suggested. Selected Reference...
Abstract
Field metallography and replication were performed on a type 316 stainless steel column in diglycol amine vacuum service to determine the cause of visible OD pitting on the column in several areas above the insulation support rings. The examination revealed transgranular stress-corrosion cracking beneath the pitted areas on the OD. The likely cause of the cracking was chloride stress corrosion, with chlorides deriving from the marine atmosphere and concentrating under the insulation around the support rings. A complete insulation evaluation, including repair or replacement, was recommended to prevent chloride buildup. Painting of the steel surface with an epoxy-phenolic or epoxy-coal tar was also suggested.
Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001765
EISBN: 978-1-62708-241-9
... in the failure analysis. The corrosion products were analyzed using energy-dispersive X-ray analysis (EDAX). The failure is attributed to the ingress of water and its impoundment under the tank bottom along the periphery inside the ring wall and failure of water side epoxy coating. Various measures to prevent...
Abstract
This paper describes the investigation of a corrosion failure of bottom plates on an aboveground tank used for the storage of potable water. The tank was internally inspected for the first time after six years of service. Paint blisters and rust spots were observed on the bottom plates and first to third course shell plates. Sand blasting and repainting of the bottom plates and first course shell plates was to be used as a remedial measure. However, during the sand blasting, holes and deep pitting were observed on the bottom plates. On-site visual inspection, magnetic flux leakage (MFL) inspection, ultrasonic testing (UT), and evaluation of the external cathodic protection (CP) system were used in the failure analysis. The corrosion products were analyzed using energy-dispersive X-ray analysis (EDAX). The failure is attributed to the ingress of water and its impoundment under the tank bottom along the periphery inside the ring wall and failure of water side epoxy coating. Various measures to prevent such failures in the future are recommended.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.process.c9001493
EISBN: 978-1-62708-235-8
... between the epoxy board and copper caused the thin plating to crack. During electrical testing of a four-layer circuit board, an open electrical circuit was found between the plated through-holes. Plating discontinuity was caused by poor drilling using a dull drill with improper speed (rpm) and/or feed...
Abstract
An open electrical circuit was found between plated through-holes in a six-layer printed circuit board after thermal cycling. The copper plating was very thin in the failure area but did make an electrical contact during initial testing. During thermal cycling, differential z-expansion between the epoxy board and copper caused the thin plating to crack. During electrical testing of a four-layer circuit board, an open electrical circuit was found between the plated through-holes. Plating discontinuity was caused by poor drilling using a dull drill with improper speed (rpm) and/or feed rate as was observed by nonuniform plating and nodule formation in the plated layer. In a third example, an open electrical circuit was found in a six-layer board between two adjacent plated through-holes. A plating void was on one side of the conductor joining the two holes. Continuity was found when tested from one side of the board but lost when tested from the other. In a fourth case, an open circuit found between a plated through-hole and contact pad on a six-layer printed circuit board was caused by an etching defect.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.bldgs.c9001656
EISBN: 978-1-62708-219-8
... to sinusoidal load fluctuations at 6.7 Hz in air, 3% NaCl solution, and natural sea water are described. Reinforcement types studied included: hot-rolled mild steel bar, hot-rolled alloyed high strength bar, cold-worked high strength bar, galvanized bar of all these three types, nickel-clad bar and epoxy-coated...
Abstract
Some corrosion processes in the presence of chlorides, for steel embedded in concrete, are described and illustrated with the aid of scanning electron microscope EDXA data. Observations made of failure surfaces of reinforcements removed from the concrete beams after being subjected to sinusoidal load fluctuations at 6.7 Hz in air, 3% NaCl solution, and natural sea water are described. Reinforcement types studied included: hot-rolled mild steel bar, hot-rolled alloyed high strength bar, cold-worked high strength bar, galvanized bar of all these three types, nickel-clad bar and epoxy-coated bar.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.machtools.c0045903
EISBN: 978-1-62708-223-5
... in.) from the origin along the wall of a hydraulic-oil bleed hole. Investigation with a SEM showed corrosion pits along the bleed hole wall, but oxidation and corrosion prevented review of microfractographic details. Vacuum epoxy encapsulation, sectioning of the bleed hole, and metallographic examination...
Abstract
A 230 mm (9 in.) thick casing, fabricated from ASTM 235-55 low-carbon steel, of a 450 Mg (500 ton) extrusion press failed after 27 years of service. Initial visual examination revealed an area that exhibited multiple origins and classic beach marks radiating out approximately 75 mm (3 in.) from the origin along the wall of a hydraulic-oil bleed hole. Investigation with a SEM showed corrosion pits along the bleed hole wall, but oxidation and corrosion prevented review of microfractographic details. Vacuum epoxy encapsulation, sectioning of the bleed hole, and metallographic examination revealed a basic microstructure of pearlite and ferrite with bands of slightly finer pearlite, with a large concentration of inclusion stringers in the area of the fracture origin. Further investigation using an energy-dispersive x-ray analyzer showed high concentrations of sulfur and manganese. Thus, the failure appeared to have resulted from corrosion-assisted fatigue, and the inclusion concentration in the fracture-initiated area indicated that the chemical-composition limits for sulfur and manganese would have greatly exceeded material specifications. A higher quality steel was recommended for the replacement unit to lessen the possibility of such gross inclusion segregation and to improve the fracture toughness of the cylinder.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c0091598
EISBN: 978-1-62708-218-1
... concentrated ammonium nitrate solution. Recommendations included the cost-effective solution of applying a three-coat epoxy-type coating with a total dry thickness of 0.3 mm (0.013 in.) to the interior surfaces of the hoppers. Ammonium nitrate Epoxy Hoppers ASTM A611 ASTM A570 Intergranular fracture...
Abstract
After 10 to 20 months of service, the carbon steel hoppers on three trucks used to transport bulk ammonium nitrate prills developed extensive cracking in the upper walls. The prills were discharged from the steel hoppers using air superchargers that generated an unloading pressure of approximately 11 kPa (7 psi). Each hopper truck held from 9,100 to 11,800 kg (10 to 13 tons) of prills when fully loaded and handled approximately 90,700 kg (100 tons) per month. The walls of the hoppers were made of 2.7 mm (0.105 in.) thick flat-rolled carbon steel sheet of structural quality, conforming to ASTM A 245 (obsolete specification replaced by A 570 and A 611). Investigation (visual inspection and 100x micrographs polished and etched with nital) supported the conclusion that failure of the hoppers was the result of intergranular SCC of the sheet-steel walls because of contact with a highly concentrated ammonium nitrate solution. Recommendations included the cost-effective solution of applying a three-coat epoxy-type coating with a total dry thickness of 0.3 mm (0.013 in.) to the interior surfaces of the hoppers.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.aero.c0006402
EISBN: 978-1-62708-217-4
... to anodizing. A hot inhibited alkaline cleaner was also recommended during cleaning prior to anodizing. The panels should be dichromate sealed after anodizing. The use of deionized water was also recommended during the dichromate sealing operation. In addition, the use of an epoxy primer prior to shipment...
Abstract
New aircraft wing panels extruded from 7075-T6 aluminum exhibited an unusual pattern of circular black interrupted lines, which could not be removed by scouring or light sanding. The panels, subsequent to profiling and machining, were required to be penetrated inspected, shot peened, H2SO4 anodized, and coated with MIL-C-27725 integral fuel tank coating on the rib side. Scanning electron microscopy and microprobe analysis (both conventional energy-dispersive and Auger analyzers) showed that the anodic coating was applied over an improperly cleaned and contaminated surface. The expanding corrosion product had cracked and, in some places, had flaked away the anodized coating. The corrodent had penetrated the base aluminum in the form of subsurface intergranular attack to a depth of 0.035 mm (0.0014 in.). It was recommended that a vapor degreaser be used during cleaning prior to anodizing. A hot inhibited alkaline cleaner was also recommended during cleaning prior to anodizing. The panels should be dichromate sealed after anodizing. The use of deionized water was also recommended during the dichromate sealing operation. In addition, the use of an epoxy primer prior to shipment of the panels was endorsed. Most importantly, surveillance of the anodizing process itself was emphasized.
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
...) and Group 2 resistors. The group 2 resistor had been exposed to the heat of soldering for 90 s. Note the dark appearance of the top polymer coating. This is due to the pyrolysis, or breakdown, of the epoxy coating. 19.25× Fig. 3 Delaminated group 8 resistor that exhibited a low pushoff strength...
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
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006929
EISBN: 978-1-62708-395-9
... of a tetraglycidyl methylenedianiline/diaminodiphenyl sulfone (TGMDA/DDS) system Table 5 Effect of absorbed moisture on the physical properties of a tetraglycidyl methylenedianiline/diaminodiphenyl sulfone (TGMDA/DDS) system Components A B TGMDA, parts 100 100 BPA epoxy novolac(a), pph 8.2...
Abstract
This article provides an overview of the physics and math associated with moisture-related failures in plastic components. It develops key equations, showing how they are used to analyze the causes and effects of water uptake, diffusion, and moisture concentration in polymeric materials and resins. It explains how absorbed moisture affects a wide range of properties, including glass transition temperature, flexural and shear modulus,creep, stress relaxation, swelling, tensile and yield strength, and fatigue cracking. It provides relevant data on common polymers, resins, and fiber-resin composites.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006924
EISBN: 978-1-62708-395-9
..., and ungelled glass. Source: Ref 24 Fig. 12 Heat flow as a function of temperature at a heating rate of 10 °C/min (18 °F/min) for an epoxy-amine cured isothermally at 160 °C (320 °F). d H/ dt , measured heat flow; T g , glass transition temperature; ΔH res , residual heat of reaction; ΔH rxn...
Abstract
This article discusses the most common thermal analysis methods for thermosetting resins. These include differential scanning calorimetry, thermomechanical analysis, thermogravimetric analysis, and dynamic mechanical analysis. The article also discusses the characterization of uncured thermosetting resins as well as the curing process. Then, the techniques to characterize the physical properties of cured thermosets and composites are presented. Several examples of stress-strain curves are shown for thermosets and thermoplastic polymers.
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