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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records

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NASA NTRS1980

Incorporation of metal ions into polyimides

The effects of the incorporation of metal ions into various polyimides on polyimide properties are investigated. Polyimide films derived from 3,3',4,4'-benzophenone tetracarboxylic acid dianhydride (BDTA) 3,3'-diaminobenzophenone (m,m'-DABP), 4,4'-diaminobenzophenone (p,p'-DABP) or 4,4'-oxydianiline were prepared with the concurrent addition of approximately 20 metals in a variety of forms. In general, it is found that the films derived from BDTA + p,p'-DABP were brittle and of poor quality, with brittle films also produced in most of the BDTA + m, m'-DABP polyimides regardless of whether the added metal was hydrate or anhydrous. Thermomechanical analysis, torsional braid analysis, thermal gravimetric analysis, infrared spectral analysis and isothermal studies on many of the polyimide films produced indicate that the softening temperature is generally increased upon the addition of metal ions, at the expense of thermal stability, while no changes in chemical functionality are observed. The best system studied in regard to polymer property enhancement appears to be tri(acetylacetonato)aluminum(III) added to the m, m'-DABP polyamide, which has been found to exhibit four times the lap shear strength of the polyimide alone.

Taylor, L. T.↗

NASA NTRS1975

Annealing of aromatic polyimide precursors

A study has been made of the thermal behavior of polyimide precursors: an isomeric pair of crystals of the complex formed by p-phenylenediamine with the separated isomers of the di-isopropyl ester of pyromellitic acid. Specimens of this material were isothermally annealed in the temperature range 120 C to 170 C for periods of time up to 1 week. Although this temperature range is well below that customarily used for imidizations, the working hypothesis was that it would be more likely that a polymer embodying at least part of the precursor structure could be formed if the molecular motion was minimized to that actually required for the formation of the imide linkage. The progress of the annealing was followed by: infrared spectroscopy, differential thermal analysis, powder X-ray diffraction, and thermal gravimetric analysis. Single crystal X-ray analysis of the meta monomer yields a structure of chains of alternating acid and base and suggests that this monomer is amenable to polymerization with a minimum of geometrical disruption.

Wakelyn, N. T.↗

NASA NTRS2005

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.↗

NASA NTRS1999

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.↗

NASA NTRS1981

Flammability and Photo-Stability of Selected Polymer Systems

A systematic approach to the improvement of the flammability of epoxy resins, bisphenol-A polycarbonate poly(butylene terephthalate), and Nylon 6.6 by introducing halogens and loop functionality into the flame retardants is described. The phthalides (the loop functionality containing molecules) include 3,3-bis(4-bromophenyl)-phthalide, 3,3-bis(4-chlorophenyl)phthalide, and phenolphthalein. The phthalide containing epoxy resins are synthesized and characterized in comparison with the bisphenol-A epoxy resins in terms of flammability in the copolymer systems. The resins include diglycidyl ethers of phenolphthalein, bisphenol-A. tetrabromobisphenol-A, and tetraoromophenolphthalein. The vaporization of the phthalide additive in the polymers is observed in Thermal Gravimetric Analysis. The flame retardancy is primarily due to the presence of halogens. In the poly(butylene terephthalate) system, the cleavage of the C(sub aromatic) -B bond of the flame retardant additive enhances the crosslinking react ions between the aromatic rings resulting in an increase of char formation. In the epoxy resin systems, loop functionality contributes to char formation to a larger extent. The interaction between the epoxy resin and poly-(butylene terephthalate) follows the mechanism of insertion of the oxirane ring into the ester bond. This mechanism is studied by FT-IR. The investigation of the thermal properties of the char-forming phenol-formaldehyde resins is conducted to provide information for the systematic design of high temperature flame-resistant phenolics. NMR and FT-IR are used to characterize the oligomeric resins and the cured resins. The curing agents used in the study include formaldehyde, s-trioxane and terephthaloyl chloride. The brominated phenolic resins are found to have higher oxygen indices with lower char yields.

Lo, Jeelin↗

NASA NTRS1979

Development of economical improved thick film solar cell contact

Materials were surveyed to provide candidates for an all metal electrode paste system. These consisted of a major constituent metal powder, a low melting metal powder suitable for a liquid phase sintering medium, and a powder material suitable as an etchant for silicon dioxide at sintering temperatures. By means of thermal gravimetric analysis a suitable binder was identified for low temperature fired inks. The all metal ink concept was first demonstrated with the silver system to avoid the problems of limited process windows encountered with base metal systems. A number of solid materials capable of selectively etching silicon dioxide at modest temperatures were identified. A paste with silver fluoride was screened onto N-type silicon with 5 ohm cm resistivity. The resulting contact pads had excellent adhesion but were not electrically ohmic. Metallurgically, these contacts have equal or better grain structure as commercial inks fired at the same temperatures.

Ross, B.↗

NASA NTRS1978

Ultrathin metallized PBI paper

A study to determine the feasibility of preparing ultrathin papers with a target weight of 3.5 g/m squared from polybenzimidazole (PBI) fibrids was undertaken. Small hand sheets of target weight were fabricated. They were light brown, low density materials with sufficient strength to be readily handleable. Characterization of these sheets included strength, fold endurance, thermal gravimetric analysis in air and nitrogen and photomicrographs. Two different batches of PBI fibrids were studied and differences in fabrication performance were noted. In neither case could target weight papers be prepared using conventional paper making techniques.

Chenevey, E. C.↗

NASA NTRS1979

Development of Economical Improved Thick Film Solar Cell Contact

Ross, B.↗

NASA NTRS1979

Release-rate calorimetry of multilayered materials for aircraft seats

Multilayered samples of contemporary and improved fire resistant aircraft seat materials (foam cushion, decorative fabric, slip sheet, fire blocking layer, and cushion reinforcement layer) were evaluated for their rates of heat release and smoke generation. Top layers (decorative fabric, slip sheet, fire blocking, and cushion reinforcement) with glass fiber block cushion were evaluated to determine which materials based on their minimum contributions to the total heat release of the multilayered assembly may be added or deleted. Top layers exhibiting desirable burning profiles were combined with foam cushion materials. The smoke and heat release rates of multilayered seat materials were then measured at heat fluxes of 1.5 and 3.5 W/sq cm. Choices of contact and silicone adhesives for bonding multilayered assemblies were based on flammability, burn and smoke generation, animal toxicity tests, and thermal gravimetric analysis. Abrasion tests were conducted on the decorative fabric covering and slip sheet to ascertain service life and compatibility of layers.

Fewell, L. L.↗

NASA NTRS1980

Release-rate calorimetry of multilayered materials for aircraft seats

Multilayered samples of contemporary and improved fire-resistant aircraft seat materials (foam cushion, decorative fabric, slip sheet, fire-blocking layer, and cushion-reinforcement layer) were evaluated for their rates of heat release and smoke generation. Top layers (decorative fabric, slip sheet, fire blocking, and cushion reinforcement) with glass-fiber block cushion were evaluated to determine which materials, based on their minimum contributions to the total heat release of the multilayered assembly, may be added or deleted. Top layers exhibiting desirable burning profiles were combined with foam cushion materials. The smoke and heat-release rate of multilayered seat materials were then measured at heat fluxes of 1.5 and 3.5 W/sq cm. Choices of contact and silicon adhesives for bonding multilayered assemblies were based on flammability, burn and smoke generation, animal toxicity tests, and thermal gravimetric analysis.

Fewell, L. L.↗

NASA NTRS1980

Water-deuterium oxide exchange in polymers used in spacecraft applications

The replacement of water (H2O) by deuterium oxide (D2O) and the exchange between atmospheric water and adsorbed or absorbed D2O were investigated for the polymeric materials Kapton and Mylar using thermal gravimetric analysis and infrared spectroscopy. Replacement of H2O by D2O is easily accomplished. However, exposure of D2O samples to the ambient atmosphere or gases containing H2O results in rapid proton and deuteron exchange between H2O vapor and adsorbed D2O. Replacement of H2O by D2O would not be a practical solution to alleviate spectral interferences that would result from water outgassing in spacecraft orbital environments. Maintaining the materials of interest in a dehydrated state is a more reasonable approach.

Carre, D. J.↗

NASA NTRS1983

Autothermal reforming of aliphatic and aromatic hydrocarbon liquids

Results are presented from a study of the autothermal reforming of paraffins and aromatics over nickel catalysts. The trials were performed to examine the carbon products that appear when steam is passed over hydrocarbon liquids to form H2-rich gases, i.e., the autothermal process (ATR). Attention was given to n-hexane, n-tetradecane, benzene, and benzene solutions of naphthalene with reactant preheat to 1000-1150 F. The carbon-formation limit was sought as a function of the steam-to-carbon and oxygen to carbon molar ratios at constant pressure and the preheat temperatures. The catalyst bed was examined after each trial to identify the locations and types of carbon formed using SEM, thermal gravimetric analysis, and X ray diffraction techniques. The hydrocarbon fuels each had a separate temperature and reaction profile, as well as carbon formation characteristics. No carbon formation was observed in the upper layer of the reactor bed, while both gas phase and surface-grown deposits were present in the lower part. The results are concluded of use in the study of No. 2 fuel oil for ATR feedstock.

Flytzani-Stephanopoulos, M.↗

NASA NTRS1983

Rubber-toughened polyfunctional epoxies - Brominated vs nonbrominated formulated for graphite composites

A new, commercially available, trifunctional epoxy resin (tris-(hydroxyphenyl)-methane triglycidyl ether) was modified with synthetic rubber to increase the impact resistance of epoxy/graphite composites. These composites were reinforced with commercially available satin-weave carbon cloth using two formulations of epoxies (brominated and nonbrominated) containing various amounts of carboxy-terminated butadience acrylonitrile (CTBN) rubber that had been prereacted with epoxy resin. The impact resistance was determined by measuring the interlaminar shear strength of the composites after impact. The mechanical properties, such as flexural strength and modulus at room temperature and at 93 C, were also determined. Measurements were taken of the flammability and glass transition temperature (Tg); and a thermal-gravimetric analysis was made.

Nir, Z.↗

NASA NTRS1985

Organosiloxane working fluids for the liquid droplet radiator

Siloxane-based working fluids for advanced space radiators requiring direct fluid exposure to the space environment are evaluated. Isolation of five candidate fluids by vacuum distillation from existing siloxane polymers is discussed. The five fluids recovered include a polydimethylsiloxane, three phenyl-containing siloxanes, and a methylhexylsiloxane. Vapor pressures and viscosities for the five fluids are reported over the temperature range of 250 to 400 K. Use of thermal-gravimetric analysis to reliably estimate vapor pressures of 10 to the -8 power Pascals is described. Polydimethylsiloxane (PDMS) and polymethylphenylsiloxane (PMPS) are selected from the five candidate fluids based on favorable vapor pressure and viscosity, as well as perceived stability in low-Earth orbit environments. Characterization of these fluids by infrared spectroscopy, Si-29 NMR, gel-permeation chromatography, and liquid chromatography is presented. Both fluids consist of narrow molecular weight distributions, with average molecular weights of about 2500 for PDMS and 1300 for PMPS.

Buch, R. R.↗

NASA NTRS1986

Evaluation of moisture barrier coatings on carbon-phenolic SRM nozzle materials

The carbon-phenolic composite ablative material used on the Solid Rocket Motor (SRM) nozzle is known to absorb moisture from the atmosphere. This could cause problems such as pocketing during firing. Several moisture barrier coatings were tested on the SRM nozzle material. Data are presented for six of the 12 coatings to be tested. The data were obtained from immersion of coated samples in an environmental chamber at 100 F and 100% relative humidity and by using a modified TGA (thermal gravimetric analysis) technique. The TGA technique involved allowing wet nitrogen (25 C, 80% relative humidity) to flow across a small sample at about 65 cu cm per minute while continually monitoring the weight increase. These preliminary results show Kel-F-800, a material supplied by 3M Corporation to be the better moisture barrier. A second task was to collect data on the relative absorption of water and kerosene into the carbon-phenolic SRM nozzle material. These data indicate that water absorbs into the nozzle material to a much greater extent than kerosene. Thus kerosene is the more likely solvent in which to make specific gravity measurements on the SRM nozzle material.

Mcnutt, Ronald C.↗

NASA NTRS1992

Determination of the oxidative stability of perfluoropolyalkyl ethers and correlation with chemical structure

The oxidative stabilities of several perfluoropolyalkyl ethers (PFPAE) with related chemical structures were determined by thermal gravimetric analysis and correlated with their chemical structures. These results show that oxidative stability increases as the number of difluoroformal groups decreases and as trifluoromethyl substituents are added. They are also consistent with a recently proposed intramolecular disproportionation reaction mechanism involving coordination of successive ether oxygens to a Lewis acid. Since polytetrafluoroethylene contains no oxygen, it provides an indication of the upper limit to oxidative stability of PFPAE fluids. These results also show that oxidative decomposition of PFPAE fluids requires the presence of an active metal as well as air. Consequently, it may be possible to minimize decomposition and thus improve oxidative stability by passivating reactive metal surfaces.

Helmick, Larry S.↗

NASA NTRS1998

Low-Cost Production of Composite Bushings for Jet Engine Applications

The objectives of this research program were to reduce the manufacturing costs of variable stator vane bushings by 1) eliminating the expensive carbon fiber braiding operation, 2) replacing the batch mode impregnation, B-stage, and cutting operations with a continuous process, and 3) reducing the molding cycle and machining operations with injection molding to achieve near-net shapes. Braided bushings were successfully fabricated with both AMB-17XLD and AMB-TPD resin systems. The composite bushings achieved high glass transition temperature after post-cure (+300 C) and comparable weight loss to the PNM-15 bushings. ANM-17XLD bushings made with "batch-mode" molding compound (at 0.5 in. fiber length) achieved a +300 lb-force flange break strength which was superior to the continuous braided-fiber reinforced bushing. The non-MDA resin technology developed in this contract appears attractive for bushing applications that do not exceed a 300 C use temperature. Two thermoplastic polyimide resins were synthesized in order to generate injection molding compound powders. Excellent processing results were obtained at injection temperatures in excess of 300 C. Micro-tensile specimens were produced from each resin type and the Tg measurements (by TMA) for these samples were equivalent to AURUM(R). Thermal Gravimetric Analysis (TGA) conducted at 10 C/min showed that the non-MDA AMB-type polyimide thermoplastics had comparable weight loss to PMR-15 up to 500 C.

Gray, Robert A.↗

NASA NTRS2001

Covalent Sidewall Functionalization of Carbon Nanotubes

Progress of fluorination of single-wall carbon nanotubes is being reported. Covalent attachment of alkyl groups including methyl, n-butyl and n-hexyl groups to the sidewalls of single wall carbon nanotubes (SWNTs) has been achieved. Quantitative measurement of the alkylation was done by thermal gravimetric analysis. FTIR, Raman and UV-Vis-NIR were used to characterize these alkylated SWNTs. Application of these nanotubes are being investigated-fibers, composites, batteries, lubricants, etc.

Chiang, I.W.↗