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At least 73 records · Page 4

Carbon Nanotubes Growth by CVD on Graphite Fibers

Due to the superior electrical and mechanical properties of carbon nanotubes (CNT), synthesizing CNT on various substances for electronics devices and reinforced composites have been engaged in many efforts for applications. This presentation will illustrate CNT synthesized on graphite fibers by thermal CVD. On the fiber surface, iron nanoparticles as catalysts for CNT growth are coated. The growth temperature ranges from 600 to 1000 C and the pressure ranges from 100 Torr to one atmosphere. Methane and hydrogen gases with methane content of 10% to 100% are used for the CNT synthesis. At high growth temperatures (greater than or equal to 900 C), the rapid inter-diffusion of the transition metal iron on the graphite surface results in the rough fiber surface without any CNT grown on it. When the growth temperature is relative low (650-800 C), CNT with catalytic particles on the nanotube top ends are fabricated on the graphite surface. (Methane and hydrogen gases with methane content of 10% to 100% are used for the CNT synthesis.) (By measuring the samples) Using micro Raman spectroscopy in the breath mode region, single-walled or multi-walled CNT (MWCNT), depending on growth concentrations, are found. Morphology, length and diameter of these MWCNT are determined by scanning electron microscopy and Raman spectroscopy. The detailed results of syntheses and characterizations will be discussed in the presentation.

Zhu, Shen↗

Carbon Nanotubes Growth on Graphite Fibers

Carbon nanotubes (CNT) were synthesized on graphite fibers by thermal Chemical Vapor Deposition (CVD). On the fiber surface, iron nanoparticles are coated and act as catalysts for CNT growth. The growth temperature ranges from 550 to 1000 C at an ambient pressure. Methane and hydrogen gases with methane contents of 10% to 100% are used for the CNT synthesis. At high growth temperatures (greater than 800 C), the rapid inter-diffusion of the transition metal iron on the graphite surface results in a rough fiber surface with no CNT grown on the surface. When the growth temperature is relatively low (650 - 800 C), CNT are fabricated on the graphite surface with catalytic particles on the nanotube top ends. Using micro Raman spectroscopy in the breath mode region, single-walled or multi-walled CNT can be determined, depending on methane concentrations.

Zhu, Shen↗

Synthesis of optically clear polymeric materials for high temperature windows

A polymer has been developed that has excellent potential for use as windows in spacecraft as well as conventional aircraft. This polymer, phenolphthalein polycarbonate, has outstanding thermal properties, e.g., in place of melting or burning, it produces an insulating charred foam that closes off transmission of radiant heat through the window. This fact, coupled with an oxygen index of 0.43 and a 177 C tensile strength of 58 mega Newtons/sq m, makes this polymer a prime candidate for further development. Pilot plant preparation in a 20 gallon Pfaudler kettle was accomplished and large test specimens were prepared for evaluations.

Pannell, C. E.↗

Combustion of Metals in Reduced-Gravity and Extra Terrestrial Environments

The combustion of metals is a field with important practical applications in rocket propellants, high-temperature flames, and material synthesis. Also, the safe operation of metal containers in high-pressure oxygen systems and with cryogenic fuels and oxidizers remains an important concern in industry. The increasing use of metallic components in spacecraft and space structures has also raised concerns about their flammability properties and fire suppression mechanisms. In addition, recent efforts to embark on unmanned and manned planetary exploration, such as on Mars, have also renewed the interest in metal/carbon-dioxide combustion as an effective in situ resource utilization technology. In spite of these practical applications, the understanding of the combustion properties of metals remains far behind that of the most commonly used fuels such as hydrocarbons. The lack of understanding is due to the many problems unique to metal- oxidizer reactions such as: low-temperature surface oxidation prior to ignition, heterogeneous reactions, very high combustion temperatures, product condensation, high emissivity of products, and multi-phase interactions. Very few analytical models (all neglecting the influence of gravity) have been developed to predict the burning characteristics and the flame structure details. Several experimental studies attempting to validate these models have used small metal particles to recreate gravity-free conditions. The high emissivity of the flames, rapid reaction, and intermittent explosions experienced by these particles have made the gathering of any useful information on burning rates and flame structure very difficult. The use of a reduced gravity environment is needed to clarify some of the complex interactions among the phenomena described above. First, the elimination of the intrusive buoyant flows that plague all combustion phenomena is of paramount importance in metal reactions due to the much higher temperatures reached during combustion. Second, a low-gravity environment is absolutely essential to remove the destructive effect of gravity on the shape of a molten metal droplet in order to study a spherically symmetric condition with large bulk samples. The larger size of the spherical metal droplet and the longer burning times available in reduced gravity extend the spatial and temporal dimensions to permit careful probing of the flame structure and dynamics. Third, the influence of the radiative heat transfer from the solid oxides can be studied more carefully by generating a stagnant spherical shell of condensed products undisturbed by buoyancy.

Branch, M.C.↗

Effect of polymer properties and adherend surfaces on adhesion

The surface properties associated with good adhesive joints were evaluated in terms of application of adhesive bonding in aerospace technology. The physical and chemical nature was determined of Ti and Al adherend surfaces after various surface treatments, and the effects on fracture surfaces of high temperature aging, and variations in amide, anhydride, and solvent during polymer synthesis. The effects were characterized of (1) high temperature during shear strength testing, (2) fiber-reinforced composites as adherends, (3) acid/base nature of adherends, (4) aluminum powder adhesive filler, and (5) bonding pressure.

Dwight, D. W.↗

High-Throughput Top-Down and Bottom-Up Processes for Forming Single-Nanotube Based Architectures for 3D Electronics

We have developed manufacturable approaches to form single, vertically aligned carbon nanotubes, where the tubes are centered precisely, and placed within a few hundred nm of 1-1.5 micron deep trenches. These wafer-scale approaches were enabled by chemically amplified resists and inductively coupled Cryo-etchers for forming the 3D nanoscale architectures. The tube growth was performed using dc plasma-enhanced chemical vapor deposition (PECVD), and the materials used for the pre-fabricated 3D architectures were chemically and structurally compatible with the high temperature (700 C) PECVD synthesis of our tubes, in an ammonia and acetylene ambient. Tube characteristics were also engineered to some extent, by adjusting growth parameters, such as Ni catalyst thickness, pressure and plasma power during growth. Such scalable, high throughput top-down fabrication techniques, combined with bottom-up tube synthesis, should accelerate the development of PECVD tubes for applications such as interconnects, nano-electromechanical (NEMS), sensors or 3D electronics in general.

plasma-enhanced chemical vapor deposition (PECVD),↗

Carbon and Hydrogen Isotope Measurements of Alcohols and Organic Acids by Online Pyroprobe-GC-IRMS

The detection of methane in the atmosphere of Mars, combined with evidence showing widespread water-rock interaction during martian history, suggests that the production of methane on Mars may be the result of mineral surface-catalyzed CO2 and or CO reduction during Fisher-Tropsch Type (FTT) reactions. A better understanding of these reaction pathways and corresponding C and H isotope fractionations is critical to deciphering the synthesis of organic compounds produced under abiotic hydrothermal conditions. Described here is a technique for the extraction and analysis of both C and H isotopes from alcohols (C1-C4) and organic acids (C1-C6). This work is meant to provide a "proof of concept" for making meaningful isotope measurements on complex mixtures of solid-phase hydrocarbons and other intermediary products produced during high-temperature and high-pressure synthesis on mineral-catalyzed surfaces. These analyses are conducted entirely "on-line" utilizing a CDS model 5000 Pyroprobe connected to a Thermo Trace GC Ultra that is interfaced with a Thermo MAT 253 isotope ratio mass spectrometer operating in continuous flow mode. Also, this technique is designed to carry a split of the GC-separated product to a DSQ II quadrupole mass spectrometer as a means of making semi-quantitative compositional measurements. Therefore, both chemical and isotopic measurements can be carried out on the same sample.

Socki, Richard A.↗

Chemical vapor deposition of high T sub c superconductors

The results are reported of an investigation into the synthesis and properties of high temperature superconducting materials. A chemical vapor deposition apparatus was designed and built which is suitable for the preparation of multicomponent metal films This apparatus was used to prepare a series of high T sub c A-15 structure superconducting films in the binary system Nb-Ge. The effect on T sub c of a variety of substrate materials was investigated. An extensive series of ternary alloys were also prepared. Conditions allowing the brittle high T sub c (approximately 18 K) A-15 structure superconductor Nb3A1 to be prepared in a low T sub c but ductile form were found. Some of the ways that the ductile (bcc) form can be cold worked or machined are described. Measurements of rate of transformation of cold worked bcc material to the high T sub c A-15 structure with low temperature annealing are given. Preliminary measurements indicate that this material has attractive high field critical current densities.

Webb, G. W.↗

A Search for Amino Acids and Nucleobases in the Martian Meteorite Roberts Massif 04262 Using Liquid Chromatography-Mass Spectrometry

The investigation into whether Mars contains signatures of past or present life is of great interest to science and society. Amino acids and nucleobases are compounds that are essential for all known life on Earth and are excellent target molecules in the search for potential Martian biomarkers or prebiotic chemistry. Martian meteorites represent the only samples from Mars that can be studied directly in the laboratory on Earth. Here, we analyzed the amino acid and nucleobase content of the shergottite Roberts Massif (RBT) 04262 using liquid chromatography-mass spectrometry. We did not detect any nucleobases above our detection limit in formic acid extracts; however, we did measure a suite of protein and nonprotein amino acids in hot-water extracts with high relative abundances of beta-alanine and gamma-amino-eta-butyric acid. The presence of only low (to absent) levels of several proteinogenic amino acids and a lack of nucleobases suggest that this meteorite fragment is fairly uncontaminated with respect to these common biological compounds. The distribution of straight-chained amine-terminal eta-omega-amino acids in RBT 04262 resembled those previously measured in thermally altered carbonaceous meteorites. A carbon isotope ratio of -24(0/00) +/- 6(0/00) for beta-alanine in RBT 04262 is in the range of reduced organic carbon previously measured in Martian meteorites (Steele et al. 2012). The presence of eta-omega-amino acids may be due to a high temperature Fischer-Tropschtype synthesis during igneous processing on Mars or impact ejection of the meteorites from Mars, but more experimental data are needed to support these hypotheses.

Laboratory analysis↗

High-Throughput Processes and Structural Characterization of Single-Nanotube Based Devices for 3D Electronics

We have developed manufacturable approaches to form single, vertically aligned carbon nanotubes, where the tubes are centered precisely, and placed within a few hundred nm of 1-1.5 micron deep trenches. These wafer-scale approaches were enabled by chemically amplified resists and inductively coupled Cryo-etchers to form the 3D nanoscale architectures. The tube growth was performed using dc plasmaenhanced chemical vapor deposition (PECVD), and the materials used for the pre-fabricated 3D architectures were chemically and structurally compatible with the high temperature (700 C) PECVD synthesis of our tubes, in an ammonia and acetylene ambient. The TEM analysis of our tubes revealed graphitic basal planes inclined to the central or fiber axis, with cone angles up to 30 deg. for the particular growth conditions used. In addition, bending tests performed using a custom nanoindentor, suggest that the tubes are well adhered to the Si substrate. Tube characteristics were also engineered to some extent, by adjusting growth parameters, such as Ni catalyst thickness, pressure and plasma power during growth.

top-down fabrication↗

Synthesis and evaluation of C-ether formulations for use as high temperature lubricants and hydraulic fluids

The formulation and evaluation of C-ether fluids for use in the hydraulic and lubrication systems of the space shuttle and advanced air breathing engines were studied to lower the pour point of a reference C-ether from -29 C to -40 C without changing its evaporation loss. Use of disiloxanes mixed with C-ethers gave a -40 C pour point fluid with little change in the desired evaporation loss or in oxidative stability. A second -40 C pour point fluid containing only C-ethers was also developed. A screening program tested lubrication additives for C-ethers and the new fluids. Six additive packages were chosen for evaluation in 316 C bearing tests, two for evaluation in 260 C pump tests. The goal of the bearing test was a 100 hour run. The rig was a specially designed 80-mm axially loaded ball bearing. The C-ether base fluid ran only one hour at 316 C before cage wear failure occurred. The best additive blends ran 47, 94 and 100 hours. The 96 hour test gave excessive deposits. The 100 hour test had no wear failures; an unexplained loss of cage silver occurred from areas of direct fluid impingement on the cage.

Clark, F. S.↗

PETI-298 Prepared by Microwave Synthesis: Neat Resin and Composite Properties

PETI-298 is a high temperature/high performance matrix resin that is processable into composites by resin transfer molding (RTM), resin infusion and vacuum assisted RTM techniques. It is typically synthesized in a polar aprotic solvent from the reaction of an aromatic anhydride and a combination of diamines and endcapped with phenylethynylphthalic anhydride. Microwave synthesis of PETI-298 was investigated as a means to eliminate solvent and decrease reaction time. The monomers were manually mixed and placed in a microwave oven for various times to determine optimum reaction conditions. The synthetic process was subsequently scaled-up to 330g. Three batches were synthesized and combined to give 1 kg of material that was characterized for thermal and rheological properties and compared to PETI-298 prepared by the classic solution based synthetic method. The microwave synthesized PETI-298 was subsequently used to fabricate flat laminates on T650 carbon fabric by RTM. The composite panels were analyzed and mechanical properties determined and compared with those fabricated from PETI-298 prepared by the classic solution method. The microwave synthesis process and characterization of neat resin and carbon fiber reinforced composites fabricated by RTM will be presented. KEY WORDS: Resin Transfer Molding, High Temperature Polymers, Phenylethynyl Terminated Imides, Microwave Synthesis

Smith, Joseph G.↗

Free Fall Plasma-Arc Reactor for Synthesis of Carbon Nanotubes in Microgravity

High temperatures inside the plasma of a carbon arc generate strong buoyancy driven convection which has an effect on the growth and morphology of the single-walled carbon nanotubes (SWNTs). To study the effect of buoyancy on the arc process, a miniature carbon arc apparatus was designed and developed to synthesize SWNTs in a microgravity environment substantially free from buoyant convective flows. An arc reactor was operated in the 2.2- and 5.18-second drop towers at the NASA Glenn Research Center. The apparatus employed a 4 mm diameter anode and was powered by a portable battery pack capable of providing in excess of 300 amps at 30 volts to the arc for the duration of a 5-second drop. However, the principal result is that no dramatic difference in sample yield or composition was noted between normal gravity, 2.2-and 5-second long microgravity runs.

Alford, J. M.↗

Statistical Design in Isothermal Aging of Polyimide Resins

Recent developments in research on polyimides for high temperature applications have led to the synthesis of many new polymers. Among the criteria that determines their thermal oxidative stability, isothermal aging is one of the most important. Isothermal aging studies require that many experimental factors are controlled to provide accurate results. In this article we describe a statistical plan that compares the isothermal stability of several polyimide resins, while minimizing the variations inherent in high-temperature aging studies.

Sutter, James K.↗

Mechanistic Studies of Combustion and Structure Formation During Synthesis of Advanced Materials

Combustion in a variety of heterogeneous systems, leading to the synthesis of advanced materials, is characterized by high temperatures (2000-3500 K) and heating rates (up to 10(exp 6) K/s) at and ahead of the reaction front. These high temperatures generate liquids and gases which are subject to gravity-driven flow. The removal of such gravitational effects is likely to provide increased control of the reaction front, with a consequent improvement in control of the microstructure of the synthesized products. Thus, microgravity (mu-g) experiments lead to major advances in the understanding of fundamental aspects of combustion and structure formation under the extreme conditions of the combustion synthesis (CS) wave. In addition, the specific features of microgravity environment allow one to produce unique materials, which cannot be obtained under terrestrial conditions. The current research is a logic continuation of our previous work on investigations of the fundamental phenomena of combustion and structure formation that occur at the high temperatures achieved in a CS wave. Our research is being conducted in three main directions: 1) Microstructural Transformations during Combustion Synthesis of Metal-Ceramic Composites. The studies are devoted to the investigation of particle growth during CS of intermetallic-ceramic composites, synthesized from nickel, aluminum, titanium, and boron metal reactants. To determine the mechanisms of particle growth, the investigation varies the relative amount of components in the initial mixture to yield combustion wave products with different ratios of solid and liquid phases, under 1g and mu-g conditions; 2) Mechanisms of Heat Transfer during Reactions in Heterogeneous Media. Specifically, new phenomena of gasless combustion wave propagation in heterogeneous media with porosity higher than that achievable in normal gravity conditions, are being studied. Two types of mixtures are investigated: clad powders, where contact between reactants occurs within each particle, and mixtures of elemental powders, where interparticle contacts are important for the reaction; and 3) Mechanistic Studies of Phase Separation in Combustion of Thermite Systems. Studies are devoted to experiments on thermite systems (metal oxide-reducing metal) where phase separation processes occur to produce alloys with tailored compositions and properties. The separation may be either gravity-driven or due to surface forces, and systematic studies to elucidate the true mechanism are being conducted. The knowledge obtained will be used to find the most promising ways of controlling the microstructure and properties of combustion-synthesized materials. Low-gravity experiments are essential to create idealized an environment for insights into the physics and chemistry of advanced material synthesis processes.

Varma, A.↗