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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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NASA NTRS1981

Physical aging of linear and network epoxy resins

Network and linear epoxy resins principally based on the diglycidyl ether of bisphenol-A and its oligomers are prepared and studied using diamine and anhydride crosslinking agents. Rubber modified epoxies and a carbon fiber reinforced composite are also investigated. All materials display time-dependent changes when stored at temperatures below the glass transition temperature after quenching (sub-T/g/ annealing). Solvent sorption experiments initiated after different sub-T(g) annealing times demonstrate that the rate of solvent uptake can be indirectly related to the free volume of the epoxy resins. Residual thermal stresses and water are found to have little effect on the physical aging process, which affects the sub-T(g) properties of uniaxial carbon fiber reinforced epoxy material. Finally, the importance of the recovery phenomenon which affects the durability of epoxy glasses is considered.

Kong, E. S.-W.↗

NASA NTRS2001

Purification Procedures for Single-Wall Carbon Nanotubes

This report summarizes the comparison of a variety of procedures used to purify carbon nanotubes. Carbon nanotube material is produced by the arc process and laser oven process. Most of the procedures are tested using laser-grown, single-wall nanotube (SWNT) material. The material is characterized at each step of the purification procedures by using different techniques including scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), Raman, X-ray diffractometry (XRD), thermogravimetric analysis (TGA), nuclear magnetic resonance (NMR), and high-performance liquid chromatography (HPLC). The identified impurities are amorphous and graphitic carbon, catalyst particle aggregates, fullerenes, and hydrocarbons. Solvent extraction and low-temperature annealing are used to reduce the amount of volatile hydrocarbons and dissolve fullerenes. Metal catalysts and amorphous as well as graphitic carbon are oxidized by reflux in acids including HCl, HNO3 and HF and other oxidizers such as H2O2. High-temperature annealing in vacuum and in inert atmosphere helps to improve the quality of SWNTs by increasing crystallinity and reducing intercalation.

Gorelik, Olga P.↗

NASA NTRS2009

Method of synthesizing small-diameter carbon nanotubes with electron field emission properties

Carbon nanotube material having an outer diameter less than 10 nm and a number of walls less than ten are disclosed. Also disclosed are an electron field emission device including a substrate, an optionally layer of adhesion-promoting layer, and a layer of electron field emission material. The electron field emission material includes a carbon nanotube having a number of concentric graphene shells per tube of from two to ten, an outer diameter from 2 to 8 nm, and a nanotube length greater than 0.1 microns. One method to fabricate carbon nanotubes includes the steps of (a) producing a catalyst containing Fe and Mo supported on MgO powder, (b) using a mixture of hydrogen and carbon containing gas as precursors, and (c) heating the catalyst to a temperature above 950.degree. C. to produce a carbon nanotube. Another method of fabricating an electron field emission cathode includes the steps of (a) synthesizing electron field emission materials containing carbon nanotubes with a number of concentric graphene shells per tube from two to ten, an outer diameter of from 2 to 8 nm, and a length greater than 0.1 microns, (b) dispersing the electron field emission material in a suitable solvent, (c) depositing the electron field emission materials onto a substrate, and (d) annealing the substrate.

Liu, Jie↗

NASA NTRS2000

Metal Nanoparticle Aerogel Composites

We have fabricated sol-gels containing gold and silver nanoparticles. Formation of an aerogel produces a blue shift in the surface plasmon resonance as a result of the decrease in the dielectric constant of the matrix upon supercritical extraction of the solvent. However, as a result of chemical interface damping this blue shift does not obey effective medium theories. Annealing the samples in a reducing atmosphere at 400 C eliminates this discrepancy and results in narrowing and further blue shifting of the plasmon resonance. Metal particle aggregation also results in a deviation from the predictions of effective medium theories, but can be controlled through careful handling and by avoiding the use of alcohol. By applying effective medium theories to the heterogeneous interlayer surrounding each metal particle, we extend the technique of immersion spectroscopy to inhomogeneous materials characterized by spatially dependent dielectric constants, such as aerogels. We demonstrate that the shift in the surface plasmon wavelength provides the average fractional composition of each component (air and silica) in this inhomogeneous layer, i.e. the porosity of the aerogel or equivalently, for these materials, the catalytic dispersion. Additionally, the kinetics suggest that collective particle interactions in coagulated metal clusters are perturbed during silica gelation resulting in a change in the aggregate geometry.

Smith, David D.↗

NASA NTRS1989

Plasma deposited silicon nitride for indium phosphide encapsulation

The composition and the annealing characteristics of plasma-deposited silicon-nitride encapsulating films on the ion-implanted InP substrates were investigated, using two different substrate-cleaning procedures (organic solvents and HF or HIO3 solutions) prior to encapsulation. The effect of plasma deposition of silicon nitride on the InP substrates was assessed through the current-voltage characteristics of Schottky diodes. Results of XPS analyses showed that the cleaning procedure that employed HF solution left less oxygen on the InP surface than the procedure involving HIO3. No chemical interaction between the film and the substrate was observed before or after annealing.

Valco, G. J.↗

NASA NTRS1986

Polyimides containing oxyethylene units. Part 4: Polymerization of dianhydrides containing ether linkages

The development of new composite resins for various aerospace applications is attempted. Although it is highly desirable that these polymers be soluble in order to facilitate processing, they must display considerable solvent-resistance in use. A recent approach has involved the synthesis of a new series of polyimides containing flexible linkages. The polymers were prepared by the polymerization of aromatic dianhydrides with diamines containing oxyethylene linkages. For example, the polymerization of 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) with 1,2-bis(4-aminophenoxy)ethane (1a) and bis2-(4-aminophenoxy)ethylether (lb), afforded highly crystalline polyimides that were completely insoluble. However, a polyimide that was amorphous and soluble was obtained from the polymerization of BTDA and an isomer of lb, i.e., bis2-(3-aminophenoxy)ethyl ether (4b). In an attempt to obtain a soluble, amorphous polyimide that could be annealed into a crysalline state, block copolymers of 1b and 4b and BTDA were prepared. Copolymers containing less than 20 weight % 1b were soluble in organic solvents. However, these polymers did not crystallize when heated above their Tg's. Copolymers containing higher levels of 1b were semicrystalline and insoluble. The polymerization of the diamines containing oxyethylene linkages with 4,4'-oxydiphthalic anhydride (ODPA) and a new dianhydride, i.e., 4,4'-oxyethyleneoxyethyleneoxydiphthalic anhydride (OEDA) was investigated. It was postulated that the use of these more flexible dianhydrides would result in more processable polyimides.

Harris, F. W.↗

NASA NTRS2001

Tunable Optical Properties of Metal Nanoparticle Sol-Gel Composites

We demonstrate that the linear and non-linear optical properties of sol-gels containing metal nanoparticles are highly tunable with porosity. Moreover, we extend the technique of immersion spectroscopy to inhomogeneous hosts, such as aerogels, and determine rigorous bounds for the average fractional composition of each component, i.e., the porosity of the aerogel, or equivalently, for these materials, the catalytic dispersion. Sol-gels containing noble metal nanoparticles were fabricated and a significant blue-shift in the surface plasmon resonance (SPR) was observed upon formation of an aerogel, as a result of the decrease in the dielectric constant of the matrix upon supercritical extraction of the solvent. However, as a result of chemical interface damping and aggregation this blue-shift does not strictly obey standard effective medium theories. Mitigation of these complications is achieved by avoiding the use of alcohol and by annealing the samples in a reducing atmosphere.

Smith, David D.↗

NASA NTRS1987

Adhesive properties of a semi-crystalline polyimide

Adhesive and film properties of a new semi-crystalline polyimide, designated LARC-CPI, having a glass transition temperature of 222 C and a crystalline melt temperature of 350 C are presented. The films exhibited excellent resistance to solvents and strong base. Compact tension specimens from LARC-CPI moldings displayed a fracture energy of 37.8 lb/sq in. Titanium tensile shear specimens gave strengths of 6250 psi initially at 25 C, 7120 psi at 25 C after 1000 hours at 232 C, 2800 psi at 232 C after annealing for 5 hours at 300 C, and 3670 psi at 232 C after 100 hours at 316 C in air.

Hergenrother, P. M.↗

NASA NTRS2001

Organic Protomolecule Assembly in Igneous Minerals

C-H stretching bands in the infrared spectrum of single crystals of nominally high purity, laboratory-grown MgO and of natural upper mantle olivine provide an "organic" signature that closely resembles the symmetrical and asymmetrical C-H stretching modes of aliphatic -CH2- units. The C-H stretching bands indicate that H20 and CO2, dissolved in the matrix of these minerals, converted to form H2 and chemically reduced C, which in turn formed C-H entities, probably through segregation into defects such as dislocations. Heating causes the C-H bonds to pyrolyze and the C-H stretching bands to disappear, but annealing at 70 C causes them to reappear within a few days or weeks. Modeling dislocations in MgO suggests that the segregation of C can lead to Cx chains, x less than or equal to 4, with the terminal C atoms anchored to the MgO matrix by bonding to two U. Allowing H2 to react with such Cx chains leads to [O2C(CH2)2CO2] or similar precipitates. It is suggested that such Cx-Hy-Oz entities represent protomolecules from which derive the short-chain carboxylic and dicarboxylic and of the medium-chain fatty acids that have been solvent-extracted from crushed MgO and olivine single crystals, respectively. Thus it appears that the hard, dense matrix of igneous minerals represents a medium in which protomolecular units can be assembled. During weathering of rocks the protomolecular units turn into complex organic molecules. These processes may have provided stereochemically constrained organics to the early Earth that were crucial to the emergence of Life.

Freund, Friedemann↗