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differential thermal analysis
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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
..., viscosity average molecular weight Quasi-elastic light scattering (QELS) Macromolecular particle diameter, diffusion coefficient Particle size in dilute dispersions, molecular aggregation Differential thermal analysis (DTA) Glass transition temperatures, T g ; melt/crystallization temperatures...
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.a0006945
EISBN: 978-1-62708-395-9
... for assembly design for manufacturing and assembly diglycidyl ether of bisphenol A digital image correlation dynamic key curve dynamic mechanical analysis degree of freedom dioctyl phthalate differential scanning calorimetry differential thermal analysis de ection temperature under load drop weight index poly...
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c9001593
EISBN: 978-1-62708-234-1
... utilized included scanning electron microscopy, Fourier transform infrared spectroscopy, differential scanning calorimetry, thermomechanical analysis, and melt flow rate determination. It was the conclusion of the investigation that the part failed via brittle fracture, with evidence also indicating low...
Abstract
A failure analysis was conducted on a flow-sensing device that had cracked while in service. The polysulfone sensor body cracked radially, adjacent to a molded-in steel insert. This article describes the investigative methods used to conduct the failure analysis. The techniques utilized included scanning electron microscopy, Fourier transform infrared spectroscopy, differential scanning calorimetry, thermomechanical analysis, and melt flow rate determination. It was the conclusion of the investigation that the part failed via brittle fracture, with evidence also indicating low cycle fatigue associated with cyclic temperature changes from normal service. The design of the part and the material selection were significant contributing factors because of stresses induced during molding, physical aging of the amorphous polysulfone resin, and the substantial differential in coefficients of thermal expansion between the polysulfone and the mating steel insert.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c9001901
EISBN: 978-1-62708-218-1
... Abstract Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were used to analyze an automotive polyoxymethylene (POM) sensor housing that was depolymerizing during service. It was found that a combination of heat, oxygen, and sulfuric acid attacked and caused premature...
Abstract
Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were used to analyze an automotive polyoxymethylene (POM) sensor housing that was depolymerizing during service. It was found that a combination of heat, oxygen, and sulfuric acid attacked and caused premature failure of the part. POM should not be selected for automotive applications where elevated temperatures and acidic environments can exist. If exposure to acid is suspected, sodium bicarbonate should be applied to neutralize the surrounding environment, followed by copious quantities of water, and repeated until no effervescence is observed.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.9781627081801
EISBN: 978-1-62708-180-1
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0006548
EISBN: 978-1-62708-180-1
... growth rate DBTT ductile-to-ductile transition tempera- ture diam diameter DIN Deutsche Industrie-Normen DMA dynamic mechanical analysis DoD Department of Defense DPFAD deformation plasticity failure assess- ment diagram DSC differential scanning calorimetry DTA differential thermal analysis E Young s...
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.aero.c0046972
EISBN: 978-1-62708-217-4
... halfway from the leading edge to the trailing edge on the concave surface before ultimate failure occurred in dynamic tension. Analysis (including visual inspection, SEM, and 250x/500x micrographic examination) supported the conclusions that the blades failed due to thermal fatigue. Recommendations...
Abstract
During disassembly of an engine that was to be modified, a fractured turbine blade was found. When the fracture was examined at low magnification, it was observed that a fatigue fracture had originated on the concave side of the leading edge and had progressed slightly more than halfway from the leading edge to the trailing edge on the concave surface before ultimate failure occurred in dynamic tension. Analysis (including visual inspection, SEM, and 250x/500x micrographic examination) supported the conclusions that the blades failed due to thermal fatigue. Recommendations included application of a protective coating to the blades, provided the coating was sufficiently ductile to avoid cracking during operation to prevent surface oxidation. Such a coating would also alleviate thermal differentials, provided the thermal conductivity of the coating exceeded that of the base metal. It was also determined that directionally solidified blades could minimize thermal fatigue cracking by eliminating intersection of grain boundaries with the surface. However, this improvement would be more costly than applying a protective coating.
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
... Fig. 48 Tensile stress-strain curves for typical plastics Fig. 49 Loading geometry for ASTM D648 heat-deflection temperature test Abstract This article discusses the most common thermal analysis methods for thermosetting resins. These include differential scanning calorimetry...
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.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006849
EISBN: 978-1-62708-395-9
..., Annual Book of ASTM Standards , ASTM International 40. “ Standard Test Method for Transition Temperatures of Polymers by Thermal Analysis ,” D 3418, Annual Book of ASTM Standards , ASTM International Differential Scanning Calorimetry Thermomechanical Testing Thermogravimetric Analysis...
Abstract
This article addresses some established protocols for characterizing thermoplastics and whether they are homogeneous resins, alloyed, or blended compositions or highly modified thermoplastic composites. It begins with a discussion on characterizing mechanical, rheological, and thermal properties of polymer. This is followed by a section describing molecular weight determination using viscosity measurements. Next, the article discusses the use of cone and plate and parallel plate geometries in melt rheology. It then reviews the processes involved in the analysis of thermoplastic resins by chromatography. Finally, the article covers three operations of thermoanalysis, namely differential scanning calorimetry, thermogravimetric analysis, and thermomechanical testing.
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
... identification, contamination, degradation, chemical contact Differential scanning calorimetry (DSC) Heat of fusion, melting point, glass transition temperature, heat capacity Material identification, level of crystallinity, aging/degradation, thermal history Thermogravimetric analysis (TGA) Weight loss...
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.
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
... on a DuPont 993 thermal analyzer equipped with appropriate differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) modules. Analyses performed in air at a 5 °C/min (9 °F/min) heatup Polymer candidate First significant endotherm or T g obtained on postcured film using DSC...
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 Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.chem.c0048772
EISBN: 978-1-62708-220-4
... through the fireside edge of the fracture surface. Scale was observed over most of the crack path which acted as a stress raiser. The effect of the oxide was magnified during thermal cycles because of differential thermal expansion, with the steel having a greater expansion coefficient than the scale...
Abstract
A return bend (made from ASTM A213, grade T11, ferritic steel) from a triolefin-unit heater ruptured after two years in service. The unit operated at 2410 kPa, with a hydrocarbon feed stream (85% propylene) entering at 260 to 290 deg C and leaving at 425 to 480 deg C. The fracture was found to terminate at the welds that joined the bend to the pipeline. A high concentration of both small and large inclusions was exhibited by the metallographic examination of the steel near the fracture. Branched cracks similar to those produced by stress corrosion of steel were observed in a section through the fireside edge of the fracture surface. Scale was observed over most of the crack path which acted as a stress raiser. The effect of the oxide was magnified during thermal cycles because of differential thermal expansion, with the steel having a greater expansion coefficient than the scale. It was recommended that material that is intended for critical applications where failure cannot be tolerated should be non-destructively examined.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.matlhand.c0047321
EISBN: 978-1-62708-224-2
... than its mounts and would contract onto them. Brittle fracture of the brake drum occurred as a result of thermal contraction of the drum web against the clutch mount and the disk. The ID of the drum web was enlarged sufficiently to allow for clearance between the web and the clutch mount and disk...
Abstract
A 58.4 cm (23 in.) diam heavy-duty brake drum component of a cable-wound winch broke into two pieces during a shutdown period. Average service life of these drums was two weeks; none had failed by wear. The drums were sand cast from ductile iron. During haul-out, the cable on the cable drum drove the brake drum, and resistance was provided by brake bands applied to the outside surface of the brake drum. Friction during heavy service was sufficient to heat the brake drum, clutch mount, and disk to a red color. Examination of the assembly indicated that the brake drum would cool faster than its mounts and would contract onto them. Brittle fracture of the brake drum occurred as a result of thermal contraction of the drum web against the clutch mount and the disk. The ID of the drum web was enlarged sufficiently to allow for clearance between the web and the clutch mount and disk at a temperature differential of up to 555 deg C (1000 deg F). With the adoption of this procedure, brake drums failed by wear only.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.power.c9001011
EISBN: 978-1-62708-229-7
... of failure involved overheating of the Cr-Mo outlet tubes, heavy oxidation, oxide cracking on thermal cycling, thermal fatigue cracking plus oxidation, creep-controlled crack growth, and rapid plastic deformation and rupture. This failure was indicative of excess temperature of the steam coming from the heat...
Abstract
After some 87,000 h of operation, failure took place in the bend of a steam pipe connecting a coil of the third superheater of a steam generator to the outlet steam collector. The unit operated at 538 deg C and 135 kPa, producing 400 t/h of steam. The 2.25Cr-1Mo steel pipe in which failure took place was 50.8 mm in diam with a nominal wall thickness of 8 mm. It connected to the AISI 321 superheater tube by means of a butt weld and was one of 46 such parallel connecting tubes. The Cr-Mo tubing was situated outside the heat transfer zone of the superheater. The overall sequence of failure involved overheating of the Cr-Mo outlet tubes, heavy oxidation, oxide cracking on thermal cycling, thermal fatigue cracking plus oxidation, creep-controlled crack growth, and rapid plastic deformation and rupture. This failure was indicative of excess temperature of the steam coming from the heat transfer zone of the coil. It showed that many damage mechanisms may combine in the transition from fracture initiation to final failure. The presence of grain boundary sliding as an indication of creep damage was useful in the characterization of the stress level as high and showed that the process of creep was not operative throughout the life of the equipment.
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
... 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...
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 Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006757
EISBN: 978-1-62708-295-2
... Molecular weight (MW) and molecular weight distribution (MWD) using light scattering as well as other secondary methods Methods of thermal analysis Differential scanning calorimetry (DSC) and differential thermal analysis Thermomechanical analysis Dynamic mechanical analysis Thermogravimetric...
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 Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003522
EISBN: 978-1-62708-180-1
... methods Methods of thermal analysis Differential scanning calorimetry (DSC) and differential thermal analysis (DTA) Thermomechanical analysis Dynamic mechanical analysis Thermogravimetric analysis X-ray diffraction (XRD) analysis Further details of polymer characterization...
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.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.power.c0091655
EISBN: 978-1-62708-229-7
... surface analysis would be required to clarify this point. The role of the tight crevice between the safe-end and the thermal sleeve thus comes into question. It was considered unlikely that a classical differential aeration cell could develop in the crevice in the uniform high-purity water environment...
Abstract
Cracking occurred in an ASME SB166 Inconel 600 safe-end forging on a nuclear reactor coolant water recirculation nozzle while it was in service. The safe-end was welded to a stainless-steel-clad carbon steel nozzle and a type 316 stainless steel transition metal pipe segment. An Inconel 600 thermal sleeve was welded to the safe-end, and a repair weld had obviously been made on the outside surface of the safe-end to correct a machining error. Initial visual examination of the safe-end disclosed that the cracking extended over approximately 85 deg of the circular circumference of the piece. Investigation (visual inspection, on-site radiographic inspection, limited ultrasonic inspection, chemical analysis, 53x metallographic cross sections and SEM images etched in 8:1 phosphoric acid) supported the conclusion that the cracking mechanism was intergranular SCC. No recommendations were made.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.homegoods.c0090445
EISBN: 978-1-62708-222-8
... identified, but a likely source appeared to be the use of improper regrind. Contaminants Electric appliances Embrittlement Housings Molding resins Protective covers Stress cracking Thermal analysis Acrylonitrile-butadiene-styrene Brittle fracture Numerous protective covers, used...
Abstract
Numerous protective covers, used in conjunction with an electrical appliance, failed during assembly with the mating components. The failures were traced to a particular production lot of the covers and occurred during insertion of the screws into the corresponding bosses. The parts had been injection molded from an ABS resin to which regrind was routinely added. Inspection of both the failed covers and retained parts, which exhibited normal behavior during assembly, included visual inspection, micro-FTIR in the ATR mode, and analysis using DSC. The FTIR results indicated the presence of contaminant material exclusively within the ABS resin used to mold the failed covers, and the thermograms suggested contamination with a PBT resin. Further TGA analysis showed the contamination was estimated to account for approximately 23% of the failed cover material. The conclusion was that the appliance covers failed via brittle fracture associated with stress overload. The failures, which occurred under normal assembly conditions, were attributed to embrittlement of the molded parts, due to contamination of the ABS resin with a high level of PBT. The source of the PBT resin was not positively identified, but a likely source appeared to be the use of improper regrind.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.chem.c9001736
EISBN: 978-1-62708-220-4
... the plates and the pipe. The creep damage failure was attributed to repeated relaxation cycles of very high thermal stresses of resulting from the periodic shutdowns, temperature fluctuations during service, or both. This failure emphasized the information available from an evaluation of the operative creep...
Abstract
Leakage was detected at the welds between stiffening plates and the pipe in a transfer line carrying butane and related petrochemical compounds. The line and reinforcing rings were of AISI 316 stainless steel, the pipe being of 508 mm diam and 6.25 mm wall thickness. The design temperature and pressure were 621 deg C and 2.75 kPa, respectively, while the operating conditions were 579 deg C and 1.03 kPa. The line was insulated. Failure occurred after approximately 90,000 h of operation, shutdowns being approximately two per annum. The cracking occurred at the toe of welds between the plates and the pipe. The creep damage failure was attributed to repeated relaxation cycles of very high thermal stresses of resulting from the periodic shutdowns, temperature fluctuations during service, or both. This failure emphasized the information available from an evaluation of the operative creep mechanism, namely grain boundary sliding, relating to the periodic nature of the loading, with high residual stresses being present.
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