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NASA NTRS1974

Spacecraft nitrogen generation

Two spacecraft nitrogen (N2) generation systems based on the catalytic dissociation of hydrazine (N2H4) were evaluated. In the first system, liquid N2H4 is catalytically dissociated to yield an N2 and hydrogen (H2) gas mixture. Separation of the N2/H2 gas mixture to yield N2 and a supply of H2 is accomplished using a polymer-electrochemical N2/H2 separator. In the second system, the N2/H2 gas mixture is separated in a two-stage palladium/silver (Pd/Ag) N2/H2 separator. The program culminated in the successful design, fabrication, and testing of a N2H4 catalytic dissociator, a polymer-electrochemical N2/H2 separator, and a two-stage Pd/Ag N2/H2 separator. The hardware developed was sized for an N2 delivery rate of 6.81 kg/d (15lb/day). Experimental results demonstrated that both spacecraft N2 generation systems are capable of producing 6.81 kg/d (15lb/day) of 99.9% pure N2 at a pressure greater than or equal to 1035 kN/m(2) (150 psia).

Marshall, R. D.↗

NASA NTRS1985

Formulation/cure technology for ultrahigh molecular weight silphenylene-siloxane polymers

Molecular weights above one million were achieved for methylvinylsilphenylene-siloxane terpolymers using a two-stage polymerization technique which was successfully scaled up to 200 grams. The resulting polymer was vulcanized by two different formulations and compared to an identically formulated commercial methylvinyl silicone on the basis of ultimate strength, Young's modulus, percent elongation at failure, and tear strength. Relative thermal/oxidative stabilities of the elastomers were assessed by gradient and isothermal thermogravimetric analyses performed in both air and nitrogen. The experimental elastomer exhibited enhanced thermal/oxidative stability and possed equivalent or superior mechanical properties. The effect of variations in prepolymer molecular weight on mechanical properties was also investigated.

Hundley, N. H.↗

NASA NTRS1989

The composition of heavy molecular ions inside the ionopause of Comet Halley

The RPA2-PICCA instrument aboard the Giotto spacecraft obtained 10-210 amu mass spectral of cold thermal molecular ions in the coma of Comet Halley. The dissociation products of the long chain formaldehyde polymer polyoxymethylene (POM) have recently been proposed as the dominant complex molecules in the coma of Comet Halley; however, POM alone cannot account for all of the features of the high resolution spectrum. An important component of the dust at Comet Halley is particles highly enriched in carbon, hydrogen, oxygen, and nitrogen relative to the composition of carbonaceous chondrites. Since this dust could be a source for the heavy molecules observed by PICCA, a search was conducted for other chemical species by determining all the molecules with mass between 20 and 120 amu which can be made from the relatively abundant C, H, O, and N, without regard to chemical structure.

Mitchell, David L.↗

NASA NTRS1982

Carbon, hydrogen and nitrogen isotopes in solvent-extractable organic matter from carbonaceous chondrites

CCl4 and CH3OH solvent extractions were performed on the Murray, Murchison, Orgueil and Renazzo carbonaceous chondrites. Delta-D values of +300-+500% are found in the case of the CH3OH-soluble organic matter. The combined C, H and N isotope data makes it unlikely that the CH3OH-soluble components are derivable from, or simply related to, the insoluble organic polymer found in the same meteorites. A relation between the event that formed hydrous minerals in CI1 and CM2 meteorites and the introduction of water- and methanol-soluble organic compounds is suggested. Organic matter soluble in CCl4 has no N, and delta-C-13 values are lower than for CH3OH-soluble phases. It is concluded that there either are large isotopic fractionations for carbon and hydrogen between different soluble organic phases, or the less polar components are partially of terrestrial origin.

Becker, R. H.↗

NASA NTRS1996

Imide oligomers endcapped with phenylethynyl phthalic anhydrides and polymers therefrom

Controlled molecular weight phenylethynyl terminated imide oligomers (PETIs) have been prepared by the cyclodehydration of precursor phenylethynyl terminated amic acid oligomers. Amino terminated amic acid oligomers are prepared from the reaction of dianhydride(s) with an excess of diamine(s) and subsequently endcapped with phenylethynyl phthalic anhydride(s) (PEPA). The polymerizations are carried out in polar aprotic solvents such as N-methyl-2-pyrrolidinone or N,N-dimethylacetamide under nitrogen at room temperature. The amic acid oligomers are subsequently cyclodehydrated either thermally or chemically to the corresponding imide oligomers. Direct preparation of PETIs from the reaction of dianhydride(s) with an excess of diamine(s) and endcapped with phenylethynyl phthalic anhydride(s) has been performed in m-cresol. Phenylethynyl phthalic anhydrides are synthesized by the palladium catalyzed reaction of phenylacetylene with bromo substituted phthalic anhydrides in triethylamine. These new materials exhibit excellent properties and are potentially useful as adhesives, coatings, films, moldings and composite matrices.

Hergenrother, Paul M.↗

NASA NTRS1973

The effect of oxygen concentration on the boundary lubricating characteristics of an unformulated C-ether to 300 C

The effect of oxygen concentration on the boundary lubricating characteristics of an unformulated C-ether was studied with the use of a ball-on disk sliding-friction apparatus. Results were compared with those obtained with a polyphenyl ether. Experimental conditions included oxygen concentrations ranging from 20 percent (air) to 0.001 percent (nitrogen), a load of 1 kilogram, a sliding speed of 17 meters per minute, and disk temperatures ranging from 20 to 300 C (77 to 572 F). The C-ether yielded better boundary lubricating characteristics than did the polyphenyl ether in air and nitrogen over most of the temperature range. The C-ether exhibited lower wear at high oxygen levels (10 to 20 percent O2) from 25 to 200 C (77 to 392 F) and at low oxygen levels (0.001 to 1.0 percent O2) from 200 to 300 C (392 to 572 F). Friction polymer was observed around the wear scars of most test specimens. Friction polymer generation and its effect on wear are discussed in light of current theories.

Jones, W. R., Jr.↗

NASA NTRS1990

Carbon-rich particles in Comet Halley

The majority of particles detected in the coma of Comet Halley contain carbon atoms; many of these grains appear to consist preponderately or only of light elements. These light-element particles may be composed of organic compounds. Of the possible combinations of the elements hydrogen, carbon, nitrogen, and oxygen, numerous examples are found of particles containing the combinations (H,C,O,N), (H,C,N), (H,C,O), and (H,C). These results may bear on the recent detection of polyoxymethylene fragments, the observation of cyanojets (CN patterns consistent with release from solid particles), the possible presence of cyanopolyacetylenes or HCN polymer and the make-up of the CHON particles. If cometary matter could reach the surface of the earth without complete disruption, these diverse organic and mixed particles could create unique microenvironments, possibly with significant or even pivotal prebiotic chemical activity. Here a speculative insight into possible relationships between carbon in comets and carbon in life is given, as well as a brief overview of on-going analysis of data from the highly successful Particle Impact Analyzer (PIA) experiment flown on the Giotto spacecraft for the flyby of Comet Halley (development and implementation of PIA was under the direction of J. Kissel of the Max Planck Institute for Kernphysik, Heidelberg). PIA is a time-of-flight analyzer which obtains mass spectra of ions from individual particles impacting on a Pt-Ag foil target within the instrument.

Clark, Benton C.↗

NASA NTRS2012

Radiation Shielding Materials Containing Hydrogen, Boron, and Nitrogen: Systematic Computational and Experimental Study

The key objectives of this study are to investigate, both computationally and experimentally, which forms, compositions, and layerings of hydrogen, boron, and nitrogen containing materials will offer the greatest shielding in the most structurally robust combination against galactic cosmic radiation (GCR), secondary neutrons, and solar energetic particles (SEP). The objectives and expected significance of this research are to develop a space radiation shielding materials system that has high efficacy for shielding radiation and that also has high strength for load bearing primary structures. Such a materials system does not yet exist. The boron nitride nanotube (BNNT) can theoretically be processed into structural BNNT and used for load bearing structures. Furthermore, the BNNT can be incorporated into high hydrogen polymers and the combination used as matrix reinforcement for structural composites. BNNT's molecular structure is attractive for hydrogen storage and hydrogenation. There are two methods or techniques for introducing hydrogen into BNNT: (1) hydrogen storage in BNNT, and (2) hydrogenation of BNNT (hydrogenated BNNT). In the hydrogen storage method, nanotubes are favored to store hydrogen over particles and sheets because they have much larger surface areas and higher hydrogen binding energy. The carbon nanotube (CNT) and BNNT have been studied as potentially outstanding hydrogen storage materials since 1997. Our study of hydrogen storage in BNNT - as a function of temperature, pressure, and hydrogen gas concentration - will be performed with a hydrogen storage chamber equipped with a hydrogen generator. The second method of introducing hydrogen into BNNT is hydrogenation of BNNT, where hydrogen is covalently bonded onto boron, nitrogen, or both. Hydrogenation of BN and BNNT has been studied theoretically. Hyper-hydrogenated BNNT has been theoretically predicted with hydrogen coverage up to 100% of the individual atoms. This is a higher hydrogen content than possible with hydrogen storage; however, a systematic experimental hydrogenation study has not been reported. A combination of the two approaches may be explored to provide yet higher hydrogen content. The hydrogen containing BNNT produced in our study will be characterized for hydrogen content and thermal stability in simulated space service environments. These new materials systems will be tested for their radiation shielding effectiveness against high energy protons and high energy heavy ions at the HIMAC facility in Japan, or a comparable facility. These high energy particles simulate exposure to SEP and GCR environments. They will also be tested in the LaRC Neutron Exposure Laboratory for their neutron shielding effectiveness, an attribute that determines their capability to shield against the secondary neutrons found inside structures and on lunar and planetary surfaces. The potential significance is to produce a radiation protection enabling technology for future exploration missions. Crew on deep space human exploration missions greater than approximately 90 days cannot remain below current crew Permissible Exposure Limits without shielding and/or biological countermeasures. The intent of this research is to bring the Agency closer to extending space missions beyond the 90-day limit, with 1 year as a long-term goal. We are advocating a systems solution with a structural materials component. Our intent is to develop the best materials system for that materials component. In this Phase I study, we have shown, computationally, that hydrogen containing BNNT is effective for shielding against GCR, SEP, and neutrons over a wide range of energies. This is why we are focusing on hydrogen containing BNNT as an innovative advanced concept. In our future work, we plan to demonstrate, experimentally, that hydrogen, boron, and nitrogen based materials can provide mechanically strong, thermally stable, structural materials with effective radiation shielding against GCR, SEP, and neutrons.

Radiation↗

NASA NTRS1971

Development of organic non-flammable spacecraft potting, encapsulating and conformal coating compounds

The overall program objective was to develop a flexible compound which not only functioned in a manned aerospace environment as an effective electrical insulation, but whose flammability characteristics in 16.5 psia, 60% oxygen/40% nitrogen were evidenced by rapid self-extinguishment and minimal thermal (pyrolysis) degradation. The following polymeric matrices were examined in depth: fluoroelastomers, modified fluoroelastomers, silicone RTV's, and modified silicone and fluorosilicone RTV's. Almost none of these systems burned in air, but all burned in 6.2 psia oxygen. Inorganic, organic, and inorganic/organic additives were evaluated in conjunction with these polymers in order to achieve the required survival in the 16.5 psia 60/40 environment. Depending upon formulations, it was possible to achieve nonflammable products when tested in the 1/4 in. x 1/4 in. x 1 in. configuration, even up to and including 16.5 psia oxygen. However, in order to assure this level of flame resistance, it was found necessary to heavily load the matrix with the additives. This resulted in a significant reduction in mechanical properties and large increases in viscosities. Optimization of formulations to obtain a suitable balance between these properties and flammability resistance led to the final selection of Formulation 387 as the primary system.

Lieberman, S. L.↗

NASA NTRS1998

Long Term Degradation of Polyimide Composites

The durability of polymer matrix composites exposed to harsh environments is a major concern. Surface degradation and damage are observed in polyimide composites used in air at 125-300 C. It is believed that diffusion of oxygen into the material and oxidative chemical reactions are responsible. Previous work has characterized and modeled diffusion behavior, and thermogravimetric analyses (TGAS) have been carried out in nitrogen, air, and oxygen to provide quantitative information on thermal and oxidative reactions. However, the model developed using these data did not successfully extrapolate TGA data down to conditions seen in service. A test program that focuses on lower temperatures and makes use of isothermal tests was undertaken to achieve a better understanding of the degradation reactions under use conditions. A new, low-cost technique was developed to collect chemical degradation data for isothermal tests lasting over 200 hours in the temperature range 125-300 C. Results indicate complex behavior not captured by the previous model, including the presence of weight-adding reactions. Weight gain reactions dominated in the 125-225 C temperature range, while weight loss reactions dominated beyond 225 C. The data obtained from isothermal tests and earlier TGAs is used to develop an advanced model of the material behavior.

Patekar, Kaustubh A.↗

NASA NTRS1991

Photochemical reactions of cyanoacetylene and dicyanoacetylene: Possible processes in Titan's atmosphere

Titan has an atmosphere which is subject to dramatic chemical evolution due mainly to the dramatic effect of the UV flux from the Sun. The energetic solar photons and other particles are converting the methane-nitrogen atmosphere into the unsaturated carbon compounds observed by the Voyager probes. These same solar photons are also converting some of these unsaturated reaction products into the aerosols observed in the atmosphere which obscure the view of the surface of Titan. In particular, the photochemical reactions of cyanoacetylene, dicyanoacetylene, acetylene and ethylene may result in the formation of the higher hydrocarbons and polymers which result in the aerosols observed in Titan's atmosphere. Polymers are the principal reaction products formed by irradiation of cyanoacetylene and dicyanoacetylene. Irradiation of cyanoacetylene with 185 nm of light also yields 1,3,5-tricyanobenzene while irradiation at 254 nm yields 1,2,4-tricyanobenzene and tetracyano cyclooctatetraenes. Photolyses of mixtures of cyanoacetylene and acetylene yields mono- and di- cyanobenzenes. The 1-Cyanocyclobutene is formed from the photochemical addition of cyanoacetylene with ethylene. The photolysis of dicyanoacetylene with acetylene yields 2,3-dicyano-1,3-butadiene and 1,2-dicyanobenzene. Tetracyano cyclooctatetraene products were also observed in the photolysis of mixtures of dicyanoacetylene and acetylene with 254 nm light. The 1,2-Dicyano cyclobutene is obtained from the photolysis dicyanoacetylene and ethylene. Reaction mechanisms will be proposed to explain the observed photoproducts.

Ferris, J. P.↗

NASA NTRS2000

Long Term Degradation of Resin for High Temperature Composites

The durability of polymer matrix composites exposed to harsh environments is a major concern. Surface degradation and damage are observed in polyimide composites used in air at 125 to 300 C. It is believed that diffusion of oxygen into the material and oxidative chemical reactions in the matrix are responsible. Previous work has characterized and modeled diffusion behavior, and thermogravimetric analyses (TGAs) have been carried out in nitrogen, air, and oxygen to provide quantitative information on thermal and oxidative reactions. However, the model developed using these data was not able to capture behavior seen in isothermal tests, especially those of long duration. A test program that focuses on lower temperatures and makes use of isothermal tests was undertaken to achieve a better understanding of the degradation reactions under use conditions. A new low-cost technique was developed to collect chemical degradation data for isothermal tests lasting over 200 hr in the temperature range 125 to 300 C. Results indicate complex behavior not captured by the previous TGA tests, including the presence of weight-adding reactions. Weight gain reactions dominated in the 125 to 225 C temperature range, while weight loss reactions dominated beyond 225 C. The data obtained from isothermal tests was used to develop a new model of the material behavior. This model was able to fully capture the behavior seen in the tests up to 275 C. Correlation of the current model with both isothermal data at 300 C and high rate TGA test data is mediocre. At 300 C and above, the reaction mechanisms appear to change. Attempts (which failed) to measure non-oxidative degradation indicate that oxidative reactions dominate the degradation at low temperatures. Based on this work, long term isothermal testing in an oxidative atmosphere is recommended for studying the degradation behavior of this class of materials.

Patekar, Kaustubh A.↗

NASA NTRS1991

Flow visualization of a rocket injector spray using gelled propellant simulants

A study was conducted at NASA-Lewis to compare the atomization characteristics of gelled and nongelled propellant simulants. A gelled propellant simulant composed of water, sodium hydroxide, and an acrylic acid polymer resin (as the gelling agent) was used to simulate the viscosity of an aluminum/PR-1 metallized fuel gel. Water was used as a comparison fluid to isolate the rheological effects of the water-gel and to simulate nongelled RP-1. The water-gel was injected through the central orifice of a triplet injector element and the central post of a coaxial injector element. Nitrogen gas flowed through the outer orifices of the triplet injector element and through the annulus of the coaxial injector element and atomized the gelled and nongelled liquids. Photographs of the water-gel spray patterns at different operating conditions were compared with images obtained using water and nitrogen. A laser light was used for illumination of the sprays. The results of the testing showed that the water sprays produced a finer and more uniform atomization than the water-gel sprays. Rheological analysis of the water-gel showed poor atomization caused by high viscosity of water-gel delaying the transition to turbulence.

Green, James M.↗

NASA NTRS1991

Flow visualization of a rocket injector spray using gelled propellant simulants

Green, James M.↗

NASA NTRS1987

Surface characterization in composite and titanium bonding: Carbon fiber surface treatments for improved adhesion to thermoplastic polymers

The effect of anodization in NaOH, H2SO4, and amine salts on the surface chemistry of carbon fibers was examined by X-ray photoelectron spectroscopy (XPS). The surfaces of carbon fibers after anodization in NaOH and H2SO4 were examined by scanning transmission electron microscopy (STEM), angular dependent XPS, UV absorption spectroscopy of the anodization bath, secondary ion mass spectrometry, and polar/dispersive surface energy analysis. Hercules AS-4, Dexter Hysol XAS, and Union Carbide T-300 fibers were examined by STEM, angular dependent XPS, and breaking strength measurement before and after commercial surface treatment. Oxygen and nitrogen were added to the fiber surfaces by anodization in amine salts. Analysis of the plasmon peak in the carbon 1s signal indicated that H2SO4 anodization affected the morphological structure of the carbon fiber surface. The work of adhesion of carbon fibers to thermoplastic resins was calculated using the geometric mean relationship. A correlation was observed between the dispersive component of the work of adhesion and the interfacial adhesion.

Devilbiss, T. A.↗

NASA NTRS1971

Jet-noise reduction through liquid-base foam injection.

An experimental investigation has been made of the sound-absorbing properties of liquid-base foams and of their ability to reduce jet noise. Protein, detergent, and polymer foaming agents were used in water solutions. A method of foam generation was developed to permit systematic variation of the foam density. The investigation included measurements of sound-absorption coefficents for both plane normal incidence waves and diffuse sound fields. The intrinsic acoustic properties of foam, e.g., the characteristic impedance and the propagation constant, were also determined. The sound emitted by a 1-in.-diam cold nitrogen jet was measured for subsonic (300 m/sec) and supersonic (422 m/sec) jets, with and without foam injection. Noise reductions up to 10 PNdB were measured.

Manson, L.↗

NASA NTRS2011

Polymer Electrolyte-Based Ambient Temperature Oxygen Microsensors for Environmental Monitoring

An ambient temperature oxygen microsensor, based on a Nafion polymer electrolyte, has been developed and was microfabricated using thin-film technologies. A challenge in the operation of Nafion-based sensor systems is that the conductivity of Nafion film depends on the humidity in the film. Nafion film loses conductivity when the moisture content in the film is too low, which can affect sensor operation. The advancement here is the identification of a method to retain the operation of the Nafion films in lower humidity environments. Certain salts can hold water molecules in the Nafion film structure at room temperature. By mixing salts with the Nafion solution, water molecules can be homogeneously distributed in the Nafion film increasing the film s hydration to prevent Nafion film from being dried out in low-humidity environment. The presence of organics provides extra sites in the Nafion film to promote proton (H+) mobility and thus improving Nafion film conductivity and sensor performance. The fabrication of ambient temperature oxygen microsensors includes depositing basic electrodes using noble metals, and metal oxides layer on one of the electrode as a reference electrode. The use of noble metals for electrodes is due to their strong catalytic properties for oxygen reduction. A conducting polymer Nafion, doped with water-retaining components and extra sites facilitating proton movement, was used as the electrolyte material, making the design adequate for low humidity environment applications. The Nafion solution was coated on the electrodes and air-dried. The sensor operates at room temperature in potentiometric mode, which measures voltage differences between working and reference electrodes in different gases. Repeat able responses to 21-percent oxygen in nitrogen were achieved using nitrogen as a baseline gas. Detection of oxygen from 7 to 21 percent has also been demonstrated. The room-temperature oxygen micro sensor developed has extremely low power consumption (no heating for operation, no voltage applied to the sensor, only a voltmeter is needed to measure the output), is small in size, is simple to batch-fabricate, and is high in sensor yield. It is applicable in a wide humidity range, with improved operation in low humidity after the additives were added to the Nafion film. Through further improvement and development, the sensor can be used for aerospace applications such as fuel leak detection, fire detection, and environmental monitoring.

Hunter, Gary W.↗

NASA NTRS2001

Polymer Matrix Composite Lines and Ducts

Since composite laminates are beginning to be identified for use in reusable launch vehicle propulsion systems, a task was undertaken to assess the feasibility of making cryogenic feedlines with integral flanges from polymer matrix composite materials. An additional level of complexity was added by having the feedlines be elbow shaped. Four materials, each with a unique manufacturing method, were chosen for this program. Feedlines were to be made by hand layup (HLU) with standard autoclave cure, HLU with electron beam cure, solvent-assisted resin transfer molding (SARTM), and thermoplastic tape laying (TTL). A test matrix of fill and drain cycles with both liquid nitrogen and liquid helium, along with a heat up to 250 F, was planned for each of the feedlines. A pressurization to failure was performed on any feedlines that passed the cryogenic cycling testing. A damage tolerance subtask was also undertaken in this study. The effects of foreign object impact to the materials used was assessed by cross-sectional examination and by permeability after impact testing. At the end of the program, the manufacture of the electron beam-cured feedlines never came to fruition. All of the TTL feedlines leaked heavily before any cryogenic testing, all of the SARTM feedlines leaked heavily after one cryogenic cycle. Thus, only the HLU with autoclave cure feedlines underwent the complete test matrix. They passed the cyclic testing and were pressurized to failure.

Nettles, A. T.↗