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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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS1975

Synthesis and evaluation of polymers for use in early warning fire alarm devices

Conjugated polyacetylene polymers and one condensation polyene, all containing a high degree of conjugated unsaturation, were synthesized. These polymers were characterized by chemical analysis and by thermogravimetric analysis, as well as for their film-forming capability and gas/polymer interactions. It was found that those that had a high degree of conjugated unsaturation and had resonance - stabilizing groups were very thermally stable to 200 C, e.g., poly(dicyanoacetylene), poly(ethynylferrocene) and poly(phenylacetylene); while those with labile moieties, such as poly(p-formamidophenylacetylene), among others, suffered some degradation when heated in air. When subjected to gas/polymer interaction effects, the greatest change in electrical conductance was observed when ammonia was used as the gas and poly(p-nitrophenylacetylene) was the detector. Other polymers showed similar behavior. For example, poly(ethynylcarborane), considered to be an electron acceptor also showed a change in electrical conductance when exposed to ammonia, while poly(ethynylpyridine) and poly(ethylidenepyridazine) responded to carbon monoxide. However, for "fire gases" (gases from smoldering cotton), poly(ethynylferrocene) was the most responsive. Thus, the concept of polymers with different electronegativities forming charge-transfer complexes with different gases was found to be operable.

Byrd, N. R.↗
NASA NTRS1984

Behavior of Al2O3 and SiO2 with heating in a Cl2 + CO stream

Differential thermal analysis (DTA) and Thermogravimetric analysis (TGA) were used to study the chlorination of alpha-Al2O3, gamma-Al2O3 and amorphous SiO2 in a Cl + CO stream, for the preparation of AlCl3 and SiCl4. The chlorination starting temperatures were 235 deg for Al2O3 and 680 deg for SiO2. The chlorination of alpha- and gamma-Al2O3 takes place via the formation of AlOCl as an intermediate product, and its subsequent dissociation at 480 to 560 deg, according to 3AlOCl yields AlCl3 + Al2O3. The chlorination activation energies are given for the three oxides.

Shchetinin, L. K.↗
NASA NTRS1978

Characterization of the physico-chemical properties of polymeric materials for aerospace flight

Materials intended for use in spacecraft are routinely tested at low pressures, and outgassed substances are condensed on cold surfaces at liquid nitrogen temperature, -196 C. These condensates are then analyzed by infrared spectroscopy, and gas chromotography-mass spectroscopy. The polymers were tested and allowed to outgas isothermally at 125 C and 0.000001 torr or less. Valuable information was obtained by extending the temperature range below and above 125 C. The performance of substances of interest to NASA were investigated by thermogravimetric analysis (TGA) from room temperature to 450 C or until the substance decomposed. Thermogravimetric analysis of a substance is a useful technique for studying its thermal nature in both static and dynamic thermal environments. It gives considerable insight into the stability and characterization of substances and the changes they undergo in varying thermal environments. The system is able to get pressures down to 1 micron or 0.001 torr.

Rock, M.↗
NASA NTRS1991

Isothermal thermogravimetric data acquisition analysis system

The description of an Isothermal Thermogravimetric Analysis (TGA) Data Acquisition System is presented. The system consists of software and hardware to perform a wide variety of TGA experiments. The software is written in ANSI C using Borland's Turbo C++. The hardware consists of a 486/25 MHz machine with a Capital Equipment Corp. IEEE488 interface card. The interface is to a Hewlett Packard 3497A data acquisition system using two analog input cards and a digital actuator card. The system provides for 16 TGA rigs with weight and temperature measurements from each rig. Data collection is conducted in three phases. Acquisition is done at a rapid rate during initial startup, at a slower rate during extended data collection periods, and finally at a fast rate during shutdown. Parameters controlling the rate and duration of each phase are user programmable. Furnace control (raising and lowering) is also programmable. Provision is made for automatic restart in the event of power failure or other abnormal terminations. Initial trial runs were conducted to show system stability.

Cooper, Kenneth, Jr.↗
NASA NTRS1994

ASTM E 1559 method for measuring material outgassing/deposition kinetics has applications to aerospace, electronics, and semiconductor industries

The American Society for Testing and Materials has published a new standard test method for characterizing time and temperature-dependence of material outgassing kinetics and the deposition kinetics of outgassed species on surfaces at various temperatures. This new ASTM standard, E 1559(1), uses the quartz crystal microbalance (QCM) collection measurement approach. The test method was originally developed under a program sponsored by the United States Air Force Materials Laboratory (AFML) to create a standard test method for obtaining outgassing and deposition kinetics data for spacecraft materials. Standardization by ASTM recognizes that the method has applications beyond aerospace. In particular, the method will provide data of use to the electronics, semiconductor, and high vacuum industries. In ASTM E 1559 the material sample is held in vacuum in a temperature-controlled effusion cell, while its outgassing flux impinges on several QCM's which view the orifice of the effusion cell. Sample isothermal total mass loss (TML) is measured as a function of time from the mass collected on one of the QCM's which is cooled by liquid nitrogen, and the view factor from this QCM to the cell. The amount of outgassed volatile condensable material (VCM) on surfaces at higher temperatures is measured as a function of time during the isothermal outgassing test by controlling the temperatures of the remaining QCM's to selected values. The VCM on surfaces at temperatures in between those of the collector QCM's is determined at the end of the isothermal test by heating the QCM's at a controlled rate and measuring the mass loss from the end of the QCM's as a function of time and temperature. This reevaporation of the deposit collected on the QCM's is referred to as QCM thermogravimetric analysis. Isothermal outgassing and deposition rates can be determined by differentiating the isothermal TML and VCM data, respectively, while the evaporation rates of the species can be obtained as a function of temperature by differentiating the QCM thermogravimetric analysis data.

Garrett, J. W.↗
NASA NTRS1983

Cobalt ion-containing epoxies

Varying concentrations of an organometallic cobalt complex were added to an epoxy system currently used by the aerospace industry as a composite matrix resin. Methods for combining cobalt (III) acetylacetonate with a tetraglycidyl 4,4 prime - diaminodiphenylmethane-based epoxy were investigated. The effects of increasing cobalt ion concentration on the epoxy cure were demonstrated by epoxy gel times and differential scanning calorimetry cure exotherms. Analysis on cured cobalt-containing epoxy castings included determination of glass transition temperatures by thermomechanical analysis, thermooxidative stabilities by thermogravimetric analysis, and densities in a density gradient column. Flexural strength and stiffness were also measured on the neat resin castings.

Stoakley, D. M.↗
NASA NTRS1997

Titan haze: structure and properties of cyanoacetylene and cyanoacetylene-acetylene photopolymers

The structure and morphological properties of polymers produced photochemically from the UV irradiation of cyanoacetylene and cyanoacetylene mixtures have been examined to evaluate their possible contribution to the haze layers found on Titan. A structural analysis of these polymers may contribute to our understanding of the data returned from the Huygens probe of the Cassini mission that will pass through the atmosphere of Titan in the year 2004. Infrared analysis, elemental analysis, and thermal methods (thermogravimetric analysis, thermolysis, pyrolysis) were used to examine structures of polycyanoacetylenes produced by irradiation of the gas phase HC3N at 185 and 254 nm. The resulting brown to black polymer, which exists as small particles, is believed to be a branched chain of conjugated carbon-carbon double bonds, which, on exposure to heat, cyclizes to form a graphitic structure. Similar methods of analysis were used to show that when HC3N is photolyzed in the presence of Titan's other atmospheric constituents (CH4, C2H6, C2H2, and CO), a copolymer is formed in which the added gases are incorporated as substituents on the polymer chain. Of special significance is the copolymer of HC3N and acetylene (C2H2). Even in experiments where C2H2 was absorbing nearly all of the incident photons, the ratio of C2H2 to HC3N found in the resulting polymer was only 2:1. Scanning electron microscopy was used to visually examine the polymer particles. While pure polyacetylene particles are amorphous spheres roughly 1 micrometer in diameter, polycyanoacetylenes appear to be strands of rough, solid particles slightly smaller in size. The copolymer of HC3N and C2H2 exhibits characteristics of both pure polymers. This is particularly important as pure polyacetylenes do not match the optical constants measured for Titan's atmospheric hazes. The copolymers produced by the incorporation of other minor atmospheric constituents, like HC3N, into the polyacetylenes are expected to have optical constants more comparable to those of the Titan haze.

Non-NASA Center↗
NASA NTRS1992

Effects of orbital exposure on Halar during the LDEF mission

Thermomechanical Analysis (TMA), Differential Scanning Calorimetry (DSC), and Thermogravimetric Analysis (TGA) were performed on samples of Halar exposed on the LDEF Mission for 6 years in orbit and unexposed Halar control samples. Sections 10-100 microns thick were removed from the exposed surface down to a depth of 1,000 microns through the 3 mm thick samples. The TMA and DSC results, which arise from the entire slice and not just its surface, showed no differences between the LDEF and the control samples. TMA scans were run from ambient to 300 C; results were compared by a tabulation of the glass transition temperatures. DSC scans were run from ambient to 700 C; the enthalpy of melting was compared for the samples as a function of section depth with the sample. The TGA results, which arise from the surface of the sample initially, showed a sharp increase in the topmost 50 micron section (the exposed, discolored side) in the weight loss of 170 C in oxygen. This weight loss dropped to bulk values in the range of depth of 50-200 microns. The control sample showed only a slight increase in weight loss as the top surface was approached. The LDEF Halar sample appears to be mechanically undamaged, with a surface layer which oxidizes faster as a result of orbital exposure.

Brower, William E., Jr.↗
NASA NTRS1993

Effects of orbital exposure on RTV during the LDEF mission

Thermomechanical analysis (TMA), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA) were performed on samples of RTV 511 exposed on the Long Duration Exposure Facility (LDEF) mission for 6 years in orbit and unexposed RTV 511 control samples. Slices 20- to 400-microns thick were removed from the exposed surface down to a depth of 1,500 microns through the 3-mm thick samples. The TMA and DSC results, which arise from the entire slice and not just its surface, showed no significant differences between the LDEF exposed and the control samples. TMA scans were run from ambient to 500 C; results were compared by a tabulation of the onset temperatures for flow. DSC scans were run from ambient to 600 C; no endotherms or exotherms occurred over the range observed. What appear to be glass transition temperatures were compared for the samples as a function of section depth within the sample and between the exposed and control samples. The TGA scans from 25 to 900 C, which arise from the surface of the sample initially, showed a slight increase in the top most 105-micron slice (the exposed, discolored side) in the weight loss at 600 C in oxygen. This weight loss dropped to bulk values at the next slice below the top section, a mean depth of 258 microns. The control sample also showed an increase in weight loss as the top surface was approached, but the 600 C weight losses were very inconsistent. The LDEF RTV sample appears to be mechanically undamaged, with a surface layer which oxidizes slightly faster as a result of orbital exposure.

Brower, William E., Jr.↗
NASA NTRS2015

Thermochemical Ablation Analysis of the Orion Heatshield

The Orion Multi-Purpose Crew Vehicle will one day carry astronauts to the Moon and beyond, and Orion's heatshield is a critical component in ensuring their safe return to Earth. The Orion heatshield is the structural component responsible for absorbing the intense heating environment caused by re-entry to Earth's atmosphere. The heatshield is primarily composed of Avcoat, an ablative material that is consumed during the re-entry process. Ablation is primarily characterized by two processes: pyrolysis and recession. The decomposition of in-depth virgin material is known as pyrolysis. Recession occurs when the exposed surface of the heatshield reacts with the surrounding flow. The Orion heatshield design was changed from an individually filled Avcoat honeycomb to a molded block Avcoat design. The molded block Avcoat heatshield relies on an adhesive bond to keep it attached to the capsule. In some locations on the heatshield, the integrity of the adhesive bond cannot be verified. For these locations, a mechanical retention device was proposed. Avcoat ablation was modelled in CHAR and the in-depth virgin material temperatures were used in a Thermal Desktop model of the mechanical retention device. The retention device was analyzed and shown to cause a large increase in the maximum bondline temperature. In order to study the impact of individual ablation modelling parameters on the heatshield sizing process, a Monte Carlo simulation of the sizing process was proposed. The simulation will give the sensitivity of the ablation model to each of its input parameters. As part of the Monte Carlo simulation, statistical uncertainties on material properties were required for Avcoat. Several properties were difficult to acquire uncertainties for: the pyrolysis gas enthalpy, non-dimensional mass loss rate (B´c), and Arrhenius equation parameters. Variability in the elemental composition of Avcoat was used as the basis for determining the statistical uncertainty in pyrolysis gas enthalpy and B´c. A MATLAB program was developed to allow for faster, more accurate and automated computation of Arrhenius reaction parameters. These parameters are required for a material model to be used in the CHAR ablation analysis program. This MATLAB program, along with thermogravimetric analysis (TGA) data, was used to generate uncertainties on the Arrhenius parameters for Avcoat. In addition, the TGA fitting program was developed to provide Arrhenius parameters for the ablation model of the gap filler material, RTV silicone.

Sixel, William↗
NASA NTRS1985

Optically transparent/colorless polyimides

Several series of linear aromatic polyimide films have been synthesized and characterized with the objective of obtaining maximum optical transparency. Two approaches have been used as part of this structure-property relationship study. The first approach is to vary the molecular structure so as to separate chromophoric centers and reduce electronic interactions between polymer chains to lower the intensity of color in the resulting polymer films. A second and concurrent approach is to perform polymerizations with highly purified monomers. Glass transition temperatures of thermally cured polyimide films are obtained by thermomechanical analysis and thermal decomposition temperatures are determined by thermogravimetric analysis. Transmittance UV-visible spectra of the polyimide films are compared to that of a commercial polyimide film. Fully imidized films are tested for solubility in common organic solvents. The more transparent films prepared in this study are evaluated for use on second-surface mirror thermal control coating systems. Lightly colored to colorless films are characterized by UV-visible spectroscopy before and after exposure to 300 equivalent solar hours UV irradiation and varying doses of 1 MeV electron irradiation. The effects of monomer purity, casting solvent and cure atmosphere on polyimide film transparency are also investigated.

Stclair, A. K.↗
NASA NTRS1994

Chemical and Thermal Analysis

Thermal decomposition activation energies have been determined using two methods of Thermogravimetric Analysis (TGA), with good correlation being obtained between the two techniques. Initial heating curves indicated a two-component system for Coflon (i.e. polymer plus placticizer) but a single component system for Tefzel. Two widely differing activation energies were for Coflon supported this view, 15 kcl/mol being associated with plasticizer, and 40 kcal/mol with polymer degradation. With Tefzel, values were 40-45 kcal/mol, the former perhaps being associated with a low molecular weight fraction. Appropriate acceleration factors have been determined. Thermomechanical Analysis (TMA) has shown considerable dimensional change during temperature cycles. For unaged pipe sections heating to 100 C and then holding the temperature resulted in a stable thickness increase of 2%, whereas the Coflon thickness decreased continuously, reaching -4% in 2.7 weeks. Previously strained tensile bars of Tefzel expanded on cooling during TMA. SEM performed on H2S-aged Coflon samples showed significant changes in both physical and chemical nature. The first may have resulted from explosive decompression after part of the aging process. Chemically extensive dehydrofluorination was indicated, and sulfur was present as a result of the aging. These observations indicate that chemical attack of PVDF can occur in some circumstances.

Bulluck, J. W.↗
NASA NTRS1978

Thermochemical and flammability properties of some thermoplastic and thermoset polymers - A review

The thermochemical and flammability properties of thermoplastic and thermoset polymers are discussed. The results of a thermogravimetric analysis of the polymers conducted on a DuPont 950 thermogravimetric analyzer using both nitrogen and air atmospheres are presented. Experimental data on smoke evolution are given, and the methodology for assessing the relative toxicity of the pyrolysis effluents is described. The values obtained from the flammability tests are compared with the stoichiometric char yield, and it is shown that the ignition tendency of the polymers is a linear function of the resin char yield

Kourtides, D. A.↗
NASA NTRS1982

Metal ion-containing epoxies

A variety of metallic and organometallic complexes to be used as potential additives for an epoxy used by the aerospace industry as a composite matrix resin were investigated. A total of 9 complexes were screened for compatibility and for their ability to accelerate or inhibit the cure of a highly crosslinkable epoxy resin. Methods for combining the metallic complexes with the resin were investigated, gel times recorded, and cure exotherms studied by differential scanning calorimetry. Glass transition temperatures of cured metal ion containing epoxy castings were determined by thermomechanical analysis. Thermal stabilities of the castings were determined by thermogravimetric analysis. Mechanical strength and stiffness of these doped epoxies were also measured.

Stoakley, D. M.↗
NASA NTRS2006

QTGA Analysis with Concurrent Deposition

Analysis of outgassed species behavior is often performed using QCM thermogravimetric analysis (QTGA). Prior methods are suited to laboratory testing of materials samples where the source of contaminant can be removed from the system. An approach suitable presented for use during hardware bakeout and outgassing certification is presented. An iterative process is shown to fit surface activation energies and the arrival flux for multiple species.

Hughes, David W.↗
NASA NTRS1994

Synthesis and decomposition of a novel carboxylate precursor to indium oxide

Reaction of metallic indium with benzoyl peroxide in 4-1 methylpyridine (4-Mepy) at 25 C produces an eight-coordinate mononuclear indium(III) benzoate, In(eta(sup 2)-O2CC6H5)3(4-Mepy)2 4H2O (I), in yields of up to 60 percent. The indium(III) benzoate was fully characterized by elemental analysis, spectroscopy, and X-ray crystallography; (I) exists in the crystalline state as discrete eight-coordinate molecules; the coordination sphere around the central indium atom is best described as pseudo-square pyramidal. Thermogravimetric analysis of (I) and X-ray diffraction powder studies on the resulting pyrolysate demonstrate that this new benzoate is an inorganic precursor to indium oxide. Decomposition of (I) occurs first by loss of 4-methylpyridine ligands (100 deg-200 deg C), then loss of benzoates with formation of In2O3 at 450 C. We discuss both use of carboxylates as precursors and our approach to their preparation.

Hepp, Aloysius F.↗
NASA NTRS2017

CO2 Capacity Sorbent Analysis using Volumetric Measurement Approach

In support of air revitalization system sorbent selection for future space missions, Ames Research Center (ARC) has performed CO2 capacity tests on various sorbents to complement structural strength tests from Marshall Space Flight Center (MSFC). The materials of interest are: Grace Davison Grade 544 13x, Honeywell UOP APG III, VSA-10, BASF 13x, and Grace Davison Grade 522 5A. Each sorbents CO2 capacity was measured using a Micromeritics ASAP 2020 Physisorption Volumetric Analysis machine to produce 0C, 10C, 25C, 50C, and 75C isotherms. These datasets were then extrapolated using Langmuir 3-Site and Toth isotherm models to compare with previously measured capacity data from MSFC using a thermogravimetric analysis approach. The modeling and extrapolation from ARC data correlated well with data measured at MSFC.

Air Revitalization↗
NASA NTRS1996

Chemical and Thermal Analysis

Work has included significant research in several areas aimed at further clarification of the aging and chemical failure mechanism of thermoplastics (PVDF or Tefzel) for pipes. Among the areas investigated were the crystallinity changes associated with both the Coflon and Tefzel after various simulated environmental exposures using X-Ray diffraction analysis. We have found that significant changes in polymer crystallinity levels occur as a function of the exposures. These crystallinity changes may have important consequences on the fracture, fatigue, tensile, and chemical resistance of the materials. We have also noted changes in the molecular weight distribution of the Coflon material using a dual detector Gel Permeation Analysis. Again these changes may result in variation in the mechanical and chemical properties in the material. We conducted numerous analytical studies with methods including X-Ray Diffraction, Gel Permeation Chromatography, Fourier Transform Infrared Spectroscopy, Thermogravimetric Analysis, and Differential Scanning Calorimetry. We investigated a number of aged samples of both Tefzel and Coflon that were forwarded from MERL. Pressurized tests were performed in a modified Fluid G, which we will call G2. In this case the ethylene diamine concentration was increased to 3 percent in methanol. Coflon pipe sections and powdered Coflon were exposed in pressure cells at 1700 psi at three separate test temperatures, 70 C, 110 C, and 130 C. The primary purpose of the pressure tests in Fluid G2 was to further elucidate the aging mechanism of PVDF degradation.

Bulluck, J. W.↗