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Series: ASM Failure Analysis Case Histories
Volume: 1
Publisher: ASM International
Published: 01 December 1992
DOI: 10.31399/asm.fach.v01.c9001043
EISBN: 978-1-62708-214-3
.... The cracks were covered with scale, indicating that thermal fatigue (heat cracking) had occurred. Chemical analysis confirmed that the original material was type 304 stainless steel that had been through-carburized by the formation of an endothermic gas mixture. It was recommended that plant startup...
Abstract
A 76 mm (3 in.) type 304 stainless steel tube that was used as a heat shield and water nozzle support in a hydrogen gas plant quench pot failed in a brittle manner. Visual examination of a sample from the failed tube showed that one lip of the section was eroded from service failure, whereas the opposite side exhibited a planar-type fracture. Sections were removed from the eroded area and from the opposite lip for microscopic studies and chemical analysis. The eroded edges exhibited river bed ditching, indicative of thermal fatigue. Microstructural analysis showed massive carbide formations in a martensite matrix and outlining of prior-austenite grains by a network of fine, white lines. These features indicated that the material had been transformed by carburization by the impinging gas. The outer surface exhibited a heavy scale deposit and numerous cracks that originated at the surface of the tube. The cracks were covered with scale, indicating that thermal fatigue (heat cracking) had occurred. Chemical analysis confirmed that the original material was type 304 stainless steel that had been through-carburized by the formation of an endothermic gas mixture. It was recommended that plant startup and shutdown procedures be modified to reduce or eliminate the presence of the carburizing gas mixture.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c0090442
EISBN: 978-1-62708-218-1
... endothermic transition normally associated with PBT after slow cooling. This was thought to be the result of molecular degradation, which produced shorter polymer chain lengths, therefore reducing steric hindrance. A comparison of the second heating thermograms is included in Fig. 2 . Fig. 2...
Abstract
A number of plastic sleeves used in an automotive application cracked after assembly but prior to installation into the mating components. The sleeves were specified to be injection molded from a 20% glass-fiber-reinforced polybutylene terephthalate (PBT) resin. After molding, electronic components are inserted into the sleeves, and the assembly is filled with a potting compound. Investigation of the cracked parts and some reference parts available for testing included visual inspection, micro-FTIR in the ATR mode, and analysis using DSC. Subtle spectrum differences suggested degradation of the failed part material, and the thermograms supported this. The conclusion was that the failed sleeves had cracked due to embrittlement associated with severe degradation and the corresponding molecular weight reduction. The reduction in molecular weight significantly reduced the mechanical properties of the sleeves. The cause of the degradation was not evident, but the likely source appears to be the molding operation and exposure to elevated temperature for an extended period of time.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c0090433
EISBN: 978-1-62708-218-1
... produced a greater predisposition for stress relaxation. Additives Chemical composition Clips Injection moldings Molding resins Stress relaxation Thermal analysis Wire clips Nylon 6/6 (Other, general, or unspecified) processing-related failures A production lot of plastic wire clips...
Abstract
A production lot of plastic wire clips was failing after limited service. The failures were characterized by excessive relaxation of the clips, such that the corresponding wires were no longer adequately secured in the parts. No catastrophic failures had been encountered. Parts representing an older lot, which exhibited satisfactory performance properties, were also available for reference purposes. The clips were specified to be injection molded from an impact-modified grade of nylon 6/6. However, the part drawing did not indicate a specific resin. Investigation included visual inspection, micro-FTIR in the ATR mode, and analysis using DSC. The spectrum representing the reference parts showed a relatively higher level of a hydrocarbon-based impact modifier, while the results obtained on the failed parts showed the presence of an acrylic-based modifier. Also, the reference clip thermogram showed a melting transition attributed to a hydrocarbon-based impact modifier. The conclusion was that the control and failed clips had been produced from two distinctly different resins. It appeared that the material used to produce the failed clips had different viscoelastic properties, which produced a greater predisposition for stress relaxation.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c0090451
EISBN: 978-1-62708-218-1
... the parts to temperatures above the recognized limits for PET. Brittle fracture Chemical analysis Drying Feedstock Injection moldings Molding resins Plastic jackets Thermal shock Polyethylene terephthalate Brittle fracture (Other, general, or unspecified) processing-related failures...
Abstract
Cracking occurred within the plastic jacket (injection molded from an impact-modified, 15% glass-fiber-reinforced PET resin.) of several assemblies used in a transportation application during an engineering testing regimen which involved cyclic thermal shock (exposing the parts to alternating temperatures of -40 and 180 deg C (-40 and 360 deg F)). Prior to molding, the resin had reportedly been dried at 135 deg C (275 deg F). The drying process usually lasted 6 h, but occasionally, the material was dried overnight. Comparison investigation (visual inspection, 20x SEM views, micro-FTIR, and analysis using DSC and TGA) with non-failed parts supported the conclusion that that the failure was via brittle fracture associated with the exertion of stresses that exceeded the strength of the resin as-molded caused by the disparity in the CTEs of the PET jacket and the mating steel sleeve. The drying process had exposed the resin to relatively high temperatures, which caused substantial molecular degradation, thus limiting the part's ability to withstand the stresses. The drying temperature was found to be significantly higher than the recommendation for the PET resin, and the testing itself exposed the parts to temperatures above the recognized limits for PET.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.design.c0090436
EISBN: 978-1-62708-233-4
... to produce the discrepant parts revealed that the pellets were of two general types, neither of which matched the pellets from a retained resin lot. Investigation included visual inspection, micro-FTIR in the ATR mode, and analysis using DSC. The thermograms supported the conclusion that the brittle...
Abstract
Molded plastic couplings used in an industrial application exhibited abnormally brittle properties, as compared to previously produced components. The couplings were specified to be molded from a custom-compounded glass-filled nylon 6/12 resin. An inspection of the molding resin used to produce the discrepant parts revealed that the pellets were of two general types, neither of which matched the pellets from a retained resin lot. Investigation included visual inspection, micro-FTIR in the ATR mode, and analysis using DSC. The thermograms supported the conclusion that the brittle couplings contained a significant level of contamination, polypropylene and nylon 6/6. The source of the polypropylene was likely the purging compound used to clean the compounding extruder. The origin of the nylon 6/6 resin was unknown but may represent a previously compounded resin.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003525
EISBN: 978-1-62708-180-1
... plastic resin thermogravimetric analysis thermomechanical analysis visual examination THE ULTIMATE OBJECTIVE of a failure analysis is to ascertain the mode and the cause of the failure, regardless of the material from which the part was fabricated. The investigation is performed in generally...
Abstract
This article reviews the analytical techniques most commonly used in plastic component failure analysis. These include the Fourier transform infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The descriptions of the analytical techniques are supplemented by a series of case studies that include pertinent visual examination results and the corresponding images that aid in the characterization of the failures. The article describes the methods used for determining the molecular weight of a plastic resin. It explains the use of mechanical testing in failure analysis and also describes the considerations in the selection and use of test methods.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.chem.c0090454
EISBN: 978-1-62708-220-4
.... In general, increased levels of crystallinity result in higher levels of molded-in stress and the corresponding warpage. The significant reduction in the modulus of the HDPE material, which accompanied the saturation of the resin with the aromatic hydrocarbon-based solvent, substantially decreased the creep...
Abstract
A chemical storage vessel failed while in service. The failure occurred as cracking through the vessel wall, resulting in leakage of the fluid. The tank had been molded from a high-density polyethylene (HDPE) resin. The material held within the vessel was an aromatic hydrocarbon-based solvent. Investigation (visual inspection, stereomicroscopic examination, 20x/100x SEM images, micro-FTIR in the ATR mode, and analysis using DSC and TGA) supported the conclusion that the chemical storage vessel failed via a creep mechanism associated with the exertion of relatively low stresses. The source of the stress was thought to be molded-in residual stresses associated with uneven shrinkage. This was suggested by obvious distortion evident on cutting the vessel. Relatively high specific gravity and the elevated heat of fusion indicated that the material had a high level of crystallinity. In general, increased levels of crystallinity result in higher levels of molded-in stress and the corresponding warpage. The significant reduction in the modulus of the HDPE material, which accompanied the saturation of the resin with the aromatic hydrocarbon-based solvent, substantially decreased the creep resistance of the material and accelerated the failure.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006933
EISBN: 978-1-62708-395-9
... 500× Fig. 32 Differential scanning calorimetry thermogram comparison of first heating results for the (a) molding resin and (b) failed part. An endotherm is present in the results obtained on the failed window material. The endotherm is characteristic of the melting of crystalline structure...
Abstract
This article reviews analytical techniques that are most often used in plastic component failure analysis. The description of the techniques is intended to familiarize the reader with the general principles and benefits of the methodologies, namely Fourier transform infrared spectroscopy, energy-dispersive x-ray spectroscopy, differential scanning calorimetry, thermogravimetric analysis, and dynamic mechanical analysis. The article describes the methods for molecular weight assessment and mechanical testing to evaluate plastics and polymers. The descriptions of the analytical techniques are supplemented by a series of case studies to illustrate the significance of each method. The case studies also include pertinent visual examination results and the corresponding images that aided in the characterization of the failures.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.steel.c0046998
EISBN: 978-1-62708-232-7
... and similar alloy steels in an endothermic atmosphere at about 1010 °C (1850 °F). Although the atmosphere was neutral with respect to the work, it had a carburizing potential relative to the radiant tubes. Sampling An 18-cm (7-in.) long sample piece that contained the failure region ( Fig. 1 ) was cut...
Abstract
One of 14 vertical radiant tubes (RA 333 alloy) in a heat-treating furnace failed when a hole about 5 x 12.5 cm (2 x 5 in.) corroded completely through the tube wall. The tube measured 183 cm (72 in.) in length and 8.9 cm (3 in.) in OD and had a wall thickness of about 3 mm (0.120 in.). Failure occurred where the tube passed through the refractory hearth (floor) of the furnace. Although the furnace atmosphere was neutral with respect to the work, it had a carburizing potential relative to the radiant tubes. Analysis (visual inspection, 250x spectroscopic examination of specimens etched with mixed acids, metallographic examination, and chemical analysis) supported the conclusions that the premature failure of the tube by perforation at the hearth level resulted from (1) corrosion caused by sulfur contamination from the refractory cement in contact with the tube and (2) severe local overheating at the same location. Recommendations included replacing all tubes using a low sulfur refractory cement in installation and controlling burner positioning and regulation more closely to avoid excessive heat input at the hearth level.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.homegoods.c0090448
EISBN: 978-1-62708-222-8
... and polyester. No signs of material contamination were found. The housing material was further evaluated using DSC. The thermogram obtained during the initial heating run, as shown in Fig. 2 , exhibited an endothermic transition at 253 °C (487 °F), characteristic of the melting point of a PET resin...
Abstract
Housings (being tested as part of a material conversion) from an electrical appliance failed during an engineering evaluation. They had been injection molded from a commercial polycarbonate/PET blend. Parts produced from the previous material, a nylon 6/6 resin, had consistently passed the testing regimen. Grease was applied liberally within the housing assembly during production. Investigation included visual inspection, 24x SEM images, micro-FTIR in the ATR mode, and analysis using DSC. No signs of material contamination were found, but the thermograms showed a crystallization of the PET resin. The grease present within the housing assembly, analyzed using micro-FTIR, was composed of a hydrocarbon-based oil, a phthalate-based oil, lithium stearate, and an amide-based additive. The conclusion was that the appliance housings failed through environmental stress cracking caused by a phthalate-based oil that was not compatible with the PC portion of the resin blend. Thus, the resin conversion was the root cause of the failures. Additionally, during the injection molding process the molded parts had been undercrystallized, reducing their mechanical strength. More importantly, the resin had been degraded, producing a reduction in the molecular weight and reducing both the mechanical integrity and chemical-resistance properties of the parts.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.homegoods.c0090457
EISBN: 978-1-62708-222-8
... to distinguish between these materials. Differential scanning calorimetry was used to analyze the latch material. The obtained results showed that the material underwent a single endothermic transition at approximately 165 °C (330 °F), characteristic of the melting point of a polyacetal copolymer...
Abstract
Components of a latch assembly used in a consumer safety restraint exhibited a relatively high failure rate. The failures were occurring after installation but prior to actual field use when failure could result in severe injury. Cracking occurred within retaining tabs used to secure a metal slide on an older design, whereas newer components showed no signs of failure. The latch assembly components were injection molded from an unfilled commercial grade of a polyacetal copolymer. Investigation of failed parts (including visual inspection, a specially designed proof load test, 59x SEM images, micro-FTIR in the ATR mode, and DSC/TGA/MFR analysis) showed no evidence of contamination or degradation from the molding process. The conclusion was that the parts failed via brittle fracture associated with stress overload. The stress overload was accompanied by severe apparent embrittlement resulting from a relatively high strain rate event and/or significant stress concentration. A relatively sharp corner formed by a retaining tab on the older design was shown to be a primary cause of the failures.
Series: ASM Failure Analysis Case Histories
Volume: 2
Publisher: ASM International
Published: 01 December 1993
DOI: 10.31399/asm.fach.v02.c9001328
EISBN: 978-1-62708-215-0
... Pertinent Specifications Performance of other Parts in Same or Similar Service Specimen Selection Weldments Crack Origins/Paths Testing Procedures and Results Nondestructive Evaluation Dye Penetrant Testing Visual Examination of General Physical Features Metallography...
Abstract
During 5.7 years of service, dye penetrant inspection of Inconel 800H pigtail connections regularly showed cracks at weld toes. Weld repairs were not able to prevent reoccurrence but often aggravated the condition. Samples containing small, but detectable, reducer-to-pigtail cracks showed intergranular cracks originating at weld toes and filled with oxidation product, which precluded determination of the cracking mechanism. All weldments exhibited high degrees of secondary precipitates, with original fabrication welds exhibiting higher apparent levels than repair welds. SEM/EDS analysis showed base metal grain boundary precipitates to be primarily chromium carbides, but some titanium carbides were also observed. Failure was believed to result from the synergism of thermally driven tube distortion, which resulted in over-stress, and from the intergranular oxidation products and intergranular carbides which contributed to cracking. It was recommended that stresses be reduced and /or that materials and components be changed. Refinements in welding procedures and implementation of preweld/postweld heat treatments were recommended also.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006931
EISBN: 978-1-62708-395-9
... distribution. Source: Ref 18 Fig. 16 General schematic representation of temperature rising elution fractionation (TREF). Adapted from Ref 19 Fig. 17 Schematic of differential scanning calorimetry (DSC) thermogram Fig. 18 Relationships among glass transition temperature ( T g...
Abstract
This article presents tools, techniques, and procedures that engineers and material scientists can use to investigate plastic part failures. It also provides a brief survey of polymer systems and the key properties that need to be measured during failure analysis. It describes the characterization of plastics by infrared and nuclear magnetic resonance spectroscopy, differential scanning calorimetry, differential thermal analysis, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The article also discusses the use of X-ray diffraction for analyzing crystal phases and structures in solid materials.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006923
EISBN: 978-1-62708-395-9
... … … Polyurethane (elastomer) … … … … Silicone −125 −193 … … Urethane rigid foam … … … … (a) Polymer is generally 95% or more noncrystalline. Any T m given is for remaining crystalline portion or for crystalline version. (b) Degradation temperature ( T d ) = 500 °C (930 °F). R...
Abstract
This article discusses the thermal properties of engineering plastics and elastomers with respect to chemical composition, chain configuration, and base polymer conformation as determined by thermal analysis. It describes the processing of base polymers with or without additives and their response to chemical, physical, and mechanical stresses whether as an unfilled, shaped article or as a component of a composite structure. It summarizes the basic thermal properties of thermoplastics and thermosets, including thermal conductivity, temperature resistance, thermal expansion, specific heat, and glass transition temperature. It also provides information on polyimide and bismaleimide resin systems. Representative examples of different types of engineering thermoplastics are discussed primarily in terms of structure and thermal properties.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003510
EISBN: 978-1-62708-180-1
... for a given cooling rate with time, and the cooling rate necessary to obtain martensite. The critical cooling rate is dictated by the time required to avoid formation of pearlite for the particular steel being quenched. As a general rule, a quenchant must produce a cooling rate equivalent to, or faster than...
Abstract
This article provides an overview of the effects of various material- and process-related parameters on residual stress, distortion control, cracking, and microstructure/property relationships as they relate to various types of failure. It discusses phase transformations that occur during heat treating and describes the metallurgical sources of stress and distortion during heating and cooling. The article summarizes the effect of materials and the quench-process design on distortion and cracking and details the effect of cooling characteristics on residual stress and distortion. It also provides information on the methods of minimizing distortion and tempering. The article concludes with a discussion on the effect of heat treatment processes on microstructure/property-related failures.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006932
EISBN: 978-1-62708-395-9
..., as a general class of materials, are prone to the development of internal stresses which arise during processing or during servicing when parts are exposed to environments that impose deformation and/or temperature extremes. Thermal stresses are largely a consequence of high coefficients of thermal expansion...
Abstract
Engineering plastics, as a general class of materials, are prone to the development of internal stresses which arise during processing or during servicing when parts are exposed to environments that impose deformation and/or temperature extremes. Thermal stresses are largely a consequence of high coefficients of thermal expansion and low thermal diffusivities. Although time-consuming techniques can be used to analyze thermal stresses, several useful qualitative tests are described in this article. The classification of internal stresses in plastic parts is covered. The article describes the effects of low thermal diffusivity and high thermal expansion properties, and the variation of mechanical properties with temperature. It discusses the combined effects of thermal stresses and orientation that result from processing conditions. The article also describes the effect of aging on properties of plastics. It explains the use of high-modulus graphite fibers in amorphous polymers.
Book Chapter
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006939
EISBN: 978-1-62708-395-9
... of commercial formulations Heat resistance Most are higher Generally low. High-performance varieties have excellent heat resistance. Durability (light and weather resistance) Most varieties are higher High-performance varieties have excellent durability. Acid and alkali resistance Some species...
Abstract
Polymer materials are key building blocks of the modern world, commonly used in packaging, automobiles, building materials, electronics, telecommunications, and many other industries. These commercial applications of polymeric materials would not be possible without the use of additives. This article is divided into five sections: mechanical property modifiers, physical property modifiers, biological function modifiers, processing aids, and colorants. It describes three classes of additives that are used to inhibit biological activity, six classes of mechanical property modifiers, three classes of physical property modifiers, and two classes of both colorants and processing aids.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006782
EISBN: 978-1-62708-295-2
... not participate in the electrochemical reaction. When viewed from the standpoint of partial processes of oxidation and reduction, all corrosion can be classified into a few generalized reactions. The anodic reaction in every corrosion reaction is the oxidation of a metal to its ion. This can be written...
Abstract
Corrosion is the deterioration of a material by a reaction of that material with its environment. The realization that corrosion control can be profitable has been acknowledged repeatedly by industry, typically following costly business interruptions. This article describes the electrochemical nature of corrosion and provides the typical analysis of environmental- and corrosion-related failures. It presents common methods of testing of laboratory corrosion and discusses the processes involved in the prevention of environmental- and corrosion-related failures of metals and nonmetals.