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At least 127 records · Page 7

A New DTA Method for Measuring Critical Cooling Rate for Glass Formation

A new differential thermal analysis (DTA) experimental method has been developed to determine the critical cooling rate for glass formation, R(sub c). The method, which is found especially suitable for melts that, upon cooling, have a small heat of crystallization or a very slow crystallization rate, has been verified using a 38Na2O-62SiO2 (mol%) melt with a known R(sub c) (-approx. 19 C/min), then used to determine R(sub c) for two complex lithium silicate glass forming melts. The new method is rapid, easy to conduct and yields values for R(sub c) that are in excellent agreement with the R(sub c)-values measured by standard DTA techniques.

Ray, Chandra S.↗

Thermal Properties of Lunar Regolith Simulants

Various high temperature chemical processes have been developed to extract oxygen and metals from lunar regolith. These processes are tested using terrestrial analogues of the regolith. But all practical terrestrial analogs contain H2O and/or OH(-), the presence of which has substantial impact on important system behaviors. We have undertaken studies of lunar regolith simulants to determine the limits of the simulants to validate key components for human survivability during sustained presence on the moon. Differential Thermal Analysis (DTA) yields information on phase transitions and melting temperatures. Themo-Gravimetric Analysis (TGA) with mass spectrometric (MS) determination of evolved gas species yields chemical information on various oxygenated volatiles (water, carbon dioxide, sulfur oxides, nitrogen oxides and phosphorus oxides) and their evolution temperature profiles. The DTA and TGAMS studies included JSC-1A fine, NU-LHT-2M and its proposed feed stocks: anorthosite; dunite; HQ (high quality) glass and the norite from which HQ glass is produced. Fig 1 is a data profile for anorthosite. The DTA (Fig 1a) indicates exothermic transitions at 355 and 490 C and endothermic transitions at 970 and 1235 C. Below the 355 C transition, water (Molecular Weight, MW, 18 in Fig 1c) is lost accounting for approximately 0.1% mass loss due to water removal (Fig 1b). Just above 490 C a second type of water is lost, presumably bound in lattices of secondary minerals. Between 490 and the 970 transition other volatile oxides are lost including those of hydrogen (third water type), carbon (MW = 44), sulfur (MW = 64 and 80), nitrogen (MW 30 and 46) and possibly phosphorus (MW = 79, 95 or 142). Peaks at MW = 35 and 19 may be attributable to loss of chlorine and fluorine respectively. Negative peaks in the NO (MW = 30) and oxygen (MW = 32) MS profiles may indicate the production of NO2 (MW = 46). Because so many compounds are volatilized in this temperature range quantification of the mass loss associated with individual species is difficult. Similar information will be presented for the other materials studied in this investigation.

Street, Kenneth↗

Thermal Properties of Lunar Regolith Simulants

Various high temperature chemical processes have been developed to extract oxygen and metals from lunar regolith. These processes are tested using terrestrial analogues of the regolith. But all practical terrestrial analogs contain H2O and/or OH-, the presence of which has substantial impact on important system behaviors. We have undertaken studies of lunar regolith simulants to determine the limits of the simulants to validate key components for human survivability during sustained presence on the Moon. Differential Thermal Analysis (DTA) yields information on phase transitions and melting temperatures. Thermo-Gravimetric Analysis (TGA) with Fourier Transform Infrared (FTIR) analysis provides information on evolved gas species and their evolution temperature profiles. The DTA and TGA studies included JSC-1A fine (Johnson Space Center Mare Type 1A simulant), NU-LHT-2M (National Aeronautics and Space Administration (NASA)-- United States Geological Survey (USGS)--Lunar Highlands Type 2M simulant) and its proposed feedstocks: anorthosite; dunite; high quality (HQ) glass and the norite from which HQ glass is produced. As an example, the DTA and TGA profiles for anorthosite follow. The DTA indicates exothermic transitions at 355 and 490 C and endothermic transitions at 970 and 1235 C. Below the 355 C transition, water is lost accounting for approximately 0.1 percent mass loss. Just above 490 C a second type of water is lost, presumably bound in lattices of secondary minerals along with other volatile oxides. Limited TGA-FTIR data is available at the time of this writing. For JSC-1A fine, the TGA-FTIR indicates at least two kinds of water are evolved in the 100 to 500 and the 700 to 900 C ranges. Evolution of carbon dioxide types occurs in the 250 to 545, 545 to 705, and 705 to 985 C ranges. Geologically, the results are consistent with the evolution of "water" in its several forms, CO2 from break down of secondary carbonates and magmatic, dissolved gas and glass recrystallization

Street, Kenneth W., Jr.↗

Thermal Properties of Lunar Regolith Simulants

Various high temperature chemical processes have been developed to extract oxygen and metals from lunar regolith. These processes are tested using terrestrial analogues of the regolith. But all practical terrestrial analogs contain H2O and/or OH-, the presence of which has substantial impact on important system behaviors. We have undertaken studies of lunar regolith simulants to determine the limits of the simulants to validate key components for human survivability during sustained presence on the moon. Differential Thermal Analysis (DTA) yields information on phase transitions and melting temperatures. Themo-Gravimetric Analysis (TGA) with mass spectrometric (MS) determination of evolved gas species yields chemical information on various oxygenated volatiles (water, carbon dioxide, sulfur oxides, nitrogen oxides and phosphorus oxides) and their evolution temperature profiles. The DTA and TGAMS studies included JSC-1A fine, NU-LHT-2M and its proposed feed stocks: anorthosite; dunite; HQ (high quality) glass and the norite from which HQ glass is produced. Fig 1 is a data profile for anorthosite. The DTA (Fig 1a) indicates exothermic transitions at 355 and 490 C and endothermic transitions at 970 and 1235 C. Below the 355 C transition, water (Molecular Weight, MW, 18 in Fig 1c) is lost accounting for approximately 0.1% mass loss due to water removal (Fig 1b). Just above 490 C a second type of water is lost, presumably bound in lattices of secondary minerals. Between 490 and the 970 transition other volatile oxides are lost including those of hydrogen (third water type), carbon (MW = 44), sulfur (MW = 64 and 80), nitrogen (MW 30 and 46) and possibly phosphorus (MW = 79, 95 or 142). Peaks at MW = 35 and 19 may be attributable to loss of chlorine and fluorine respectively. Negative peaks in the NO (MW = 30) and oxygen (MW = 32) MS profiles may indicate the production of NO2 (MW = 46). Because so many compounds are volatilized in this temperature range quantification of the mass loss associated with individual species is difficult. Similar information will be presented for the other materials studied in this investigation.

Street, Kenneth↗

Thermochemistry of Protective Coatings and Molten Silicate Debris

The durability of gas-turbine engine components can be significantly affected by the ingestion of siliceous particles, which can melt at high temperature and corrode protective coatings that are essential for long life requirements. The silicate debris consists mainly of CaO-MgO-Al2O3-SiO2 (CMAS) and is usually ingested by aircraft engines during and after take-off, sticking to their hot surfaces and resulting in the formation of calcium rare-earth silicate oxyapatites. The thermochemistry of coatings and their reaction products with molten silicate debris are crucial to understand in order to improve the durability of gas-turbine engines. Here we discuss results of high temperature drop solution calorimetry, drop-and-catch calorimetry (DnC) and differential thermal analysis (DTA) techniques for the thermodynamic properties of both thermal barrier coatings (TBCs) and environmental barrier coatings (EBCs) and their reaction with CMAS compositions. The enthalpies of solution of Y2Si2O7, Yb2Si2O7, 31YSZ, and 16RESZ based coatings and the oxyapatite are moderately positive. However, oxyapatite formation is only favorable over coating dissolution in terms of enthalpy for 7YSZ. The enthalpies of mixing between the coatings and the molten silicate are less exothermic for Yb2Si2O7 and CaYb4Si3O13 than for 7YSZ, indicating lower energetic stability of the latter against molten silicate corrosion. We also report for the first time the calorimetric measurements of the enthalpies of formation of rare-earth silicate based EBC coatings and oxyapatites (rare-earth, RE = Y, Yb, Gd, Dy, Er, Nd and Sm).

Costa, Gustavo↗

Use of Several Thermal Analysis Techniques on a Hypalon Paint Coating for the Solid Rocket Booster (SRB) of the Space Shuttle

White Hypalon paint is brush-applied as a moisture barrier coating over cork surfaces on each of the two Space Shuttle SRBS. Fine cracks have been observed in the Hypalon coating three times historically on laboratory witness panels, but never on flight hardware. Recent samples of the cracked and standard ("good") Hypalon were removed from cork surfaces and were tested by Thermal Gravimetric Analysis (TGA), Thermomechanical (TMA) and Differential Scanning Calorimetry (DSC) thermal analysis techniques. The TGA data showed that at 700 C, where only paint pigment solids remain, the cracked material had about 9 weight percent more material remaining than the standard material, probably indicating incomplete mixing of the paint before it was brush-applied to produce the cracked material. Use of the TMA film tension method showed that the average static modulus vs. temperature was about 3 to 6 times higher for the cracked material than for the standard material, indicating a much higher stiffness for the cracked Hypalon. The TMA data also showed than an increased coating thickness for the cracked Hypalon was not a factor in the anomaly.

Wingard, Charles D.↗

Analysis of Siderite Thermal Decomposition by Differential Scanning Calorimetry

Characterization of carbonate devolitilization has important implications for atmospheric interactions and climatic effects related to large meteorite impacts in platform sediments. On a smaller scale, meteorites contain carbonates which have witnessed shock metamorphic events and may record pressure/temperature histories of impact(s). ALH84001 meteorite contains zoned Ca-Mg-Fe-carbonates which formed on Mars. Magnetite crystals are found in the rims and cores of these carbonates and some are associated with void spaces leading to the suggestion by Brearley et al. that the crystals were produced by thermal decomposition of the carbonate at high temperature, possibly by incipient shock melting or devolitilization. Golden et al. recently synthesized spherical Mg-Fe-Ca-carbonates from solution under mild hydrothermal conditions that have similar carbonate compositional zoning to those of ALH84001. They have shown experimental evidence that the carbonate-sulfide-magnetite assemblage in ALH84001 can result from a multistep inorganic process involving heating possibly due to shock events. Experimental shock studies on calcium carbonate prove its stability to approx. 60 GPa, well in excess of the approx. 45 GPa peak pressures indicated by other shock features in ALH84001. In addition, Raman spectroscopy of carbonate globules in ALH84001 indicates no presence of CaO and MgO. Such oxide phases should be found associated with the magnetites in voids if these magnetites are high temperature shock products, the voids resulting from devolitilization of CO2 from calcium or magnesium carbonate. However, if the starting material was siderite (FeCO3), thermal breakdown of the ALH84001 carbonate at 470 C would produce iron oxide + CO2. As no documentation of shock effects in siderite exists, we have begun shock experiments to determine whether or not magnetite is produced by the decomposition of siderite within the < 45GPa pressure window and by the resultant thermal pulse to approx. 600 C experienced by ALH84001. Here, we report thermal and compositional characterization of unshocked siderite and its transition to magnetite. Additional information is contained in the original extended abstract.

Bell, M. S.↗

Differential Scanning Calorimetry and Evolved Gas Analysis at Mars Ambient Conditions Using the Thermal Evolved Gas Analyser (TEGA)

Differential Scanning Calorimetry (DSC) combined with evolved gas analysis (EGA) is a well developed technique for the analysis of a wide variety of sample types with broad application in material and soil sciences. However, the use of the technique for samples under conditions of pressure and temperature as found on other planets is one of current development and cutting edge research. The Thermal Evolved Gas Analyzer (TEGA), which was designed, built and tested at the University of Arizona's Lunar and Planetary Lab (LPL), utilizes DSC/EGA. TEGA, which was sent to Mars on the ill-fated Mars Polar Lander, was to be the first application of DSC/EGA on the surface of Mars as well as the first direct measurement of the volatile-bearing mineralogy in martian soil. Additional information is available in the original extended abstract.

Musselwhite, D. S.↗

Differential Scanning Calorimetry and Evolved Gas Analysis at Mars Ambient Conditions Using the Thermal Evolved Gas Analyzer (TEGA)

Differential Scanning Calorimetry (DSC) combined with evolved gas analysis (EGA) is a well developed technique for the analysis of a wide variety of sample types with broad application in material and soil sciences. However, the use of the technique for samples under conditions of pressure and temperature as found on other planets is one of current C development and cutting edge research. The Thermal Evolved Gas Analyzer (MGA), which was designed, built and tested at the University of Arizona's Lunar and Planetary Lab (LPL), utilizes DSC/EGA. TEGA, which was sent to Mars on the ill-fated Mars Polar Lander, was to be the first application of DSC/EGA on the surface of Mars as well as the first direct measurement of the volatile-bearing mineralogy in martian soil.

Musselwhite, D. S.↗

Use of Several Thermal Analysis Techniques on a Hypalon Paint Coating for the Solid Rocket Booster (SRB) of the Space Shuttle

White Hypalon paint is brush-applied as a moisture barrier coating over cork surfaces on each of the two Space Shuttle SRBs. Fine cracks have been observed in the Hypalon coating three times historically on laboratory witness panels, but never on flight hardware. Samples of the cracked and standard ("good") Hypalon were removed from witness panel cork surfaces, and were tested in 1998 by Thermogravimetric Analysis (TGA), TMA and Differential Scanning Calorimetry (DSC) thermal analysis techniques. The TGA data showed that at 700C, where only paint pigment solids remain, the cracked material had about 9 weight percent more material remaining than the standard material, probably indicating incomplete mixing of the paint before it was brush-applied to produce the cracked material. Use of the TMA film/fiber technique showed that the average modulus (stiffness) vs. temperature was about 3 to 6 times higher for the cracked material than for the standard material. The TMA data also showed that an increase in coating thickness for the cracked Hypalon was not a factor in the anomaly.

Wingard, Charles D.↗

Space Shuttle Columbia Aging Wiring Failure Analysis

A Space Shuttle Columbia main engine controller 14 AWG wire short circuited during the launch of STS-93. Post-flight examination divulged that the wire had electrically arced against the head of a nearby bolt. More extensive inspection revealed additional damage to the subject wire, and to other wires as well from the mid-body of Columbia. The shorted wire was to have been constructed from nickel-plated copper conductors surrounded by the polyimide insulation Kapton, top-coated with an aromatic polyimide resin. The wires were analyzed via scanning electron microscope (SEM), energy dispersive X-Ray spectroscopy (EDX), and electron spectroscopy for chemical analysis (ESCA); differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) were performed on the polyimide. Exemplar testing under laboratory conditions was performed to replicate the mechanical damage characteristics evident on the failed wires. The exemplar testing included a step test, where, as the name implies, a person stepped on a simulated wire bundle that rested upon a bolt head. Likewise, a shear test that forced a bolt head and a torque tip against a wire was performed to attempt to damage the insulation and conductor. Additionally, a vibration test was performed to determine if a wire bundle would abrade when vibrated against the head of a bolt. Also, an abrasion test was undertaken to determine if the polyimide of the wire could be damaged by rubbing against convolex helical tubing. Finally, an impact test was performed to ascertain if the use of the tubing would protect the wire from the strike of a foreign object.

McDaniels, Steven J.↗

Development of Methods of Characterizing Coal in Its Plastic State

Coal in its plastic state (typically 400-460 C) was examined by the isothermal Gieseler plastometry of seven selected coals of widely varying plastic properties. Kinetic models were proposed for the isothermal plastometric curves. Plastic behavior was compared with a variety of laboratory analyses and characterizations of these coals, including classical coal analysis; mineral analysis; microstructural analysis (extractable fractions, surface area measurement, and petrographic analysis); and thermal analysis (thermogravimetric analysis, thermomechanical analysis, and differential scanning calorimetry). The phenomenon of a sharp, large, poorly reproducible exotherm in the differential scanning calorimetric analysis of coking coals was examined. Several coal extrudates show mineral distribution, organic maceral composition and overall calorific value to be little affected by 800 F extrusion. Volatile matter and plastic properties are moderately reduced, and the network structure (as gauged by extractables) appears to be slightly degraded in the extrusion process.

Lloyd, W. G.↗

Heat storage in alloy transformations

Heats of transformation of eutectic alloys were measured for many binary and ternary systems by differential scanning calorimetry and thermal analysis. Only the relatively cheap and plentiful elements Mg, Al, Si, P, Ca, Cu, Zn were considered. A method for measuring volume change during transformation was developed using x-ray absorption in a confined sample. Thermal expansion coefficients of both solid and liquid states of aluminum and of its eutectics with copper and with silicon also were determined. Preliminary evaluation of containment materials lead to the selection of silicon carbide as the initial material for study. Possible applications of alloy PCMs for heat storage in conventional and solar central power stations, small solar receivers and industrial furnace operations are under consideration.

Birchenall, C. E.↗

Physical aging in graphite/epoxy composites

Sub-Tg annealing has been found to affect the properties of graphite/epoxy composites. The network epoxy studied was based on the chemistry of tetraglycidyl 4,4'-diamino-diphenyl methane (TGDDM) crosslinked by 4,4'-diamino-diphenyl sulfone (DDS). Differential scanning calorimetry, thermal mechanical analysis, and solid-state cross-polarized magic-angle-spinning nuclear magnetic resonance spectroscopy have been utilized in order to characterize this process of recovery towards thermodynamic equilibrium. The volume and enthalpy recovery as well as the 'thermoreversibility' aspects of the physical aging are discussed. This nonequilibrium and time-dependent behavior of network epoxies are considered in view of the increasingly wide applications of TGDDM-DDS epoxies as matrix materials of structural composites in the aerospace industry.

Kong, E. S. W.↗