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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS2014

Diamond Synthesis Employing Nanoparticle Seeds

Iron nanoparticles were employed to induce the synthesis of diamond on molybdenum, silicon, and quartz substrates. Diamond films were grown using conventional conditions for diamond synthesis by hot filament chemical vapor deposition, except that dispersed iron oxide nanoparticles replaced the seeding. This approach to diamond induction can be combined with dip pen nanolithography for the selective deposition of diamond and diamond patterning while avoiding surface damage associated to diamond-seeding methods.

Uppireddi, Kishore↗
NASA NTRS2001

Gas-Phase Combustion Synthesis of Nonoxide Nanoparticles in Microgravity

Gas-phase combustion synthesis is a promising process for creating nanoparticles for the growing nanostructure materials industry. The challenges that must be addressed are controlling particle size, preventing hard agglomerates, maintaining purity, and, if nonoxides are synthesized, protecting the particles from oxidation and/or hydrolysis during post-processing. Sodium-halide Flame Encapsulation (SFE) is a unique methodology for producing nonoxide nanoparticles that addresses these challenges. This flame synthesis process incorporates sodium and metal-halide chemistry, resulting in nanoparticles that are encapsulated in salt during the early stages of their growth in the flame. Salt encapsulation has been shown to allow control of particle size and morphology, while serving as an effective protective coating for preserving the purity of the core particles. Metals and compounds that have been produced using this technology include Al, W, Ti, TiB2, AlN, and composites of W-Ti and Al-AlN. Oxygen content in SFE synthesized nano- AlN has been measured by neutron activation analysis to be as low as 0.54wt.%, as compared to over 5wt.% for unprotected AlN of comparable size. The overall objective of this work is to study the SFE process and nano-encapsulation so that they can be used to produce novel and superior materials. SFE experiments in microgravity allow the study of flame and particle dynamics without the influence of buoyancy forces. Spherical sodium-halide flames are produced in microgravity by ejecting the halide from a spherical porous burner into a quiescent atmosphere of sodium vapor and argon. Experiments are performed in the 2.2 sec Drop Tower at the NASA-Glenn Research Center. Numerical models of the flame and particle dynamics were developed and are compared with the experimental results.

Axelbaum, R. L.↗
NASA NTRS2007

Water-Free Proton-Conducting Membranes for Fuel Cells

Poly-4-vinylpyridinebisulfate (P4VPBS) is a polymeric salt that has shown promise as a water-free proton-conducting material (solid electrolyte) suitable for use in membrane/electrode assemblies in fuel cells. Heretofore, proton-conducting membranes in fuel cells have been made from perfluorinated ionomers that cannot conduct protons in the absence of water and, consequently, cannot function at temperatures >100 C. In addition, the stability of perfluorinated ionomers at temperatures >100 C is questionable. However, the performances of fuel cells of the power systems of which they are parts could be improved if operating temperatures could be raised above 140 C. What is needed to make this possible is a solid-electrolyte material, such as P4VPBS, that can be cast into membranes and that both retains proton conductivity and remains stable in the desired higher operating temperature range. A family of solid-electrolyte materials different from P4VPBS was described in Anhydrous Proton-Conducting Membranes for Fuel Cells (NPO-30493), NASA Tech Briefs, Vol. 29, No. 8 (August 2005), page 48. Those materials notably include polymeric quaternized amine salts. If molecules of such a polymeric salt could be endowed with flexible chain structures, it would be possible to overcome the deficiencies of simple organic amine salts that must melt before being able to conduct protons. However, no polymeric quaternized amine salts have yet shown to be useful in this respect. The present solid electrolyte is made by quaternizing the linear polymer poly- 4-vinylpyridine (P4VP) to obtain P4VPBS. It is important to start with P4VP having a molecular weight of 160,000 daltons because P4VPBS made from lower-molecular-weight P4VP yields brittle membranes. In an experimental synthesis, P4VP was dissolved in methanol and then reacted with an excess of sulfuric acid to precipitate P4VPBS. The precipitate was recovered, washed several times with methanol to remove traces of acid, and dried to a white granular solid. In another synthesis, nanoparticles of silica rich with surface hydroxyl groups were added to P4VP in methanol solution, which was then reacted with excess sulfuric acid to precipitate granules of a composite that most probably had the composition (P4VPBS)-SiO2-SiO(HSO4)2. The granular P4VPBS produced in the first-mentioned synthesis was dissolved in water to make a glue-like, turbid solution; the granular P4VPBS/silica composite produced in the second-mentioned synthesis was mixed with water to make a turbid, glue-like suspension. The proportions of polymer salt to water in such preparations can be varied; it was found that approximately equal parts of water and polymer salt yield a solution or suspension amenable to further processing.

Narayanan, Sekharipuram↗
NASA NTRS2001

Flame Synthesis of Single- and Multi-Walled Carbon Nanotubes and Nanofibers

Metal-catalyzed carbon nanotubes are highly sought for a diverse range of applications that include nanoelectronics, battery electrode material, catalysis, hydrogen storage media and reinforcing agents in polymer composites. These latter applications will require vast quantities of nanotubes at competitive prices to be economically feasible. Moreover, reinforcing applications may not require ultrahigh purity nanotubes. Indeed, functionalization of nanotubes to facilitate interfacial bonding within composites will naturally introduce defects into the tube walls, lessening their tensile strength. Current methods of aerosol synthesis of carbon nanotubes include laser ablation of composite targets of carbon and catalyst metal within high temperature furnaces and decomposition of a organometallics in hydrocarbons mixtures within a tube furnace. Common to each approach is the generation of particles in the presence of the reactive hydrocarbon species at elevated temperatures. In the laser-ablation approach, the situation is even more dynamic in that particles and nanotubes are borne during the transient cooling phase of the laser-induced plasma for which the temperature far exceeds that of the surrounding hot gases within the furnace process tube. A shared limitation is that more efficient methods of nanoparticle synthesis are not readily incorporated into these approaches. In contrast, combustion can quite naturally create nanomaterials such as carbon black. Flame synthesis is well known for its commercial scalability and energy efficiency. However, flames do present a complex chemical environment with steep gradients in temperature and species concentrations. Moreover, reaction times are limited within buoyant driven flows to tens of milliseconds. Therein microgravity can greatly lessen temperature and spatial gradients while allowing independent control of flame residence times. In preparation for defining the microgravity experiments, the work presented here focuses on the effect of catalyst particle size and reactant gas in 1g.

VanderWal, R. L.↗
NASA NTRS2009

Metal-doped semiconductor nanoparticles and methods of synthesis thereof

The present invention generally relates to binary or higher order semiconductor nanoparticles doped with a metallic element, and thermoelectric compositions incorporating such nanoparticles. In one aspect, the present invention provides a thermoelectric composition comprising a plurality of nanoparticles each of which includes an alloy matrix formed of a Group IV element and Group VI element and a metallic dopant distributed within the matrix.

Ren, Zhifeng↗
NASA NTRS2016

Synthesis and Characterization of Cobalt Containing Nanoparticles on Alumina A Potential Catalyst for Gas to Liquid Fuels Production

Fisher-Tröpsch synthesis (FTS) is a century-old gas-to-liquid (GTL) technology that commonly employs cobalt (Co, on an oxide support) or iron (supported or not) species catalysts. It has been well established that the activity of the Co catalyst depends directly upon the number of surface Co atoms. The addition of promoter (mainly noble) metals has been widely utilized to increase the fraction of Co that is available for surface catalysis. Direct synthesis of Co nanoparticles is a possible alternative approach; our preliminary synthesis and characterization efforts are described. Materials were characterized by various transmission microscopies and energy dispersive spectroscopy. Tri-n-octylphosphine oxide (TOPO) and dicobalt octacarbonyl were heated under argon to a temperature of 180 deg with constant stirring for 1 hr. Quenching the reaction in toluene produced Co-containing nanoparticles with a diameter of 5 to 10 nm. Alternatively, an alumina support (SBA-200 Al2O3) was added; the reaction was further stirred and the temperature was decreased to 140 deg to reduce the rate of further growth/ripening of the nucleated Co nanoparticles. A typical size of Co-containing NPs was also found to be in the range of 5 to 10 nm. This can be contrasted with a range of 50 to 200 nm for conventionally-produced Co-Al2O3 Fischer-Tröpsch catalysts. This method shows great potential for production of highly dispersed catalysts that are either supported or unsupported.

aluminum oxides↗
NASA NTRS2008

Synthesis of Metal Nanoparticle-decorated Carbon Nanotubes under Ambient Conditions

This viewgraph presentation reviews the production of Metal Nanoparticle-decorated carbon Nanotubes. Multi-walled carbon nanotubes (MWCNTs) were efficiently decorated with metal nanoparticles (e.g. Ag, Pt, etc.) using the corresponding metal acetate in a simple mixing process without the need of chemical reagents or further processing. The conversion of acetate compounds to the corresponding metal reached over 90%, forming nanoparticles with average diameters less than 10 nm under certain conditions. The process was readily scalable allowing for the convenient preparation of multi-gram quantities of metal nanoparticle-decorated MWCNTs in a matter of a few minutes. These materials are under evaluation for a variety of electrical and catalytic applications. The preparation and characterization of these materials will be presented. The microscopic views of the processed MWCNTs are shown

Lin, Yi↗
NASA NTRS2004

A Robust and Engineerable Self-Assembling Protein Template for the Synthesis and Patterning of Ordered Nanoparticle Arrays

Self-assembling biomolecules that form highly ordered structures have attracted interest as potential alternatives to conventional lithographic processes for patterning materials. Here we introduce a general technique for patterning materials on the nanoscale using genetically modified protein cage structures called chaperonins that self-assemble into crystalline templates. Constrained chemical synthesis of transition metal nanoparticles is specific to templates genetically functionalized with poly-Histidine sequences. These arrays of materials are ordered by the nanoscale structure of the crystallized protein. This system may be easily adapted to pattern a variety of materials given the rapidly growing list of peptide sequences selected by screening for specificity for inorganic materials.

McMillan, R. Andrew↗
NASA NTRS2001

Microgravity Production of Nanoparticles of Novel Materials Using Plasma Synthesis

The research goal is to study the formation in reduced gravity of high quality nanoparticulate of novel materials using plasma synthesis. Particular emphasis will be placed on the production of powders of non-oxide materials like diamond, SiC, SiN, c-BN, etc. The objective of the study is to investigate the effect of gravity on plasma synthesis of these materials, and to determine how the microgravity synthesis can improve the quality and yield of the nanoparticles. It is expected that the reduced gravity will aid in the understanding of the controlling mechanisms of plasma synthesis, and will increase the yield, and quality of the synthesized powder. These materials have properties of interest in several industrial applications, such as high temperature load bearings or high speed metal machining. Furthermore, because of the nano-meter size of the particulate produced in this process, they have specific application in the fabrication of MEMS based combustion systems, and in the development and growth of nano-systems and nano-structures of these materials. These are rapidly advancing research areas, and there is a great need for high quality nanoparticles of different materials. One of the primary systems of interest in the project will be gas-phase synthesis of nanopowder of non-oxide materials.

Frenklach, Michael↗
NASA NTRS1999

Synthesis of Graphite Encapsulated Metal Nanoparticles and Metal Catalyzed Nanotubes

This work focuses on the growth and inception of graphite encapsulated metal nanoparticles and metal catalyzed nanotubes using combustion chemistry. Deciphering the inception and growth mechanism(s) for these unique nanostructures is essential for purposeful synthesis. Detailed knowledge of these mechanism(s) may yield insights into alternative synthesis pathways or provide data on unfavorable conditions. Production of these materials is highly desirable given many promising technological applications.

vanderWal, R. L.↗
NASA NTRS2009

Synthesis and Stability of Iron Nanoparticles for Lunar Environment Studies

Simulant of lunar dust is needed when researching the lunar environment. However, unlike the true lunar dust, today s simulants do not contain nanophase iron. Two different processes have been developed to fabricate nanophase iron to be used as part of the lunar dust simulant: (1) Sequentially treating a mixture of ferric chloride, fluorinated carbon, and soda lime glass beads at about 300 C in nitrogen, at room temperature in air, and then at 1050 C in nitrogen. The product includes glass beads that are grey in color, can be attracted by a magnet, and contain alpha-iron nanoparticles (which seem to slowly lose their lattice structure in ambient air during a period of 12 months). This product may have some similarity to the lunar glassy regolith that contains Fe(sup 0). (2) Heating a mixture of carbon black and a lunar simulant (a mixed metal oxide that includes iron oxide) at 1050 C in nitrogen. This process simulates lunar dust reaction to the carbon in a micrometeorite at the time of impact. The product contains a chemically modified simulant that can be attracted by a magnet and has a surface layer whose iron concentration increased during the reaction. The iron was found to be alpha-iron and Fe3O4 nanoparticles, which appear to grow after the fabrication process, but stabilizes after 6 months of ambient air storage.

Hung, Ching-cheh↗
NASA NTRS2009

Synthesis, Decomposition and Characterization of Fe and Ni Sulfides and Fe and CO Nanoparticles for Aerospace Applications

We describe several related studies where simple iron, nickel, and cobalt complexes were prepared, decomposed, and characterized for aeronautics (Fischer-Tropsch catalysts) and space (high-fidelity lunar regolith simulant additives) applications. We describe the synthesis and decomposition of several new nickel dithiocarbamate complexes. Decomposition resulted in a somewhat complicated product mix with NiS predominating. The thermogravimetric analysis of fifteen tris(diorganodithiocarbamato)iron(III) has been investigated. Each undergoes substantial mass loss upon pyrolysis in a nitrogen atmosphere between 195 and 370 C, with major mass losses occurring between 279 and 324 C. Steric repulsion between organic substituents generally decreased the decomposition temperature. The product of the pyrolysis was not well defined, but usually consistent with being either FeS or Fe2S3 or a combination of these. Iron nanoparticles were grown in a silica matrix with a long-term goal of introducing native iron into a commercial lunar dust simulant in order to more closely simulate actual lunar regolith. This was also one goal of the iron and nickel sulfide studies. Finally, cobalt nanoparticle synthesis is being studied in order to develop alternatives to crude processing of cobalt salts with ceramic supports for Fischer-Tropsch synthesis.

Cowen, Jonathan E.↗
NASA NTRS1999

The Features of Self-Assembling Organic Bilayers Important to the Formation of Anisotropic Inorganic Materials in Microgravity Conditions

There is a growing need for inorganic anisotropic particles in a variety of materials science applications. Structural, optical, and electrical properties can be greatly augmented by the fabrication of composite materials with anisotropic microstructures or with anisotropic particles uniformly dispersed in an isotropic matrix. Examples include structural composites, magnetic and optical recording media, photographic film, certain metal and ceramic alloys, and display technologies including flat panel displays. While considerable progress has been made toward developing an understanding of the synthesis of powders composed of monodispersed, spherical particles, these efforts have not been transferred to the synthesis of anisotropic nanoparticles. The major objective of the program is to develop a fundamental understanding of the growth of anisotropic particles at organic templates, with emphasis on the chemical and structural aspects of layered organic assemblies that contribute to the formation of anisotropic inorganic particles.

Talham, Daniel R.↗
NASA NTRS2003

Synthesis and Characterization of Chalcopyrite (CuInS2 and CuhInSe2) Colloidal Nanoparticles for Optoelectronic Applications via Low-Temperature Pyrolysis of Single-Source Precursors

Nanocrystalline (or quantum dot) materials hold potential as components of next-generation photovoltaic (PV) devices. The inclusion of quantum dots in PV devices has been proposed as a means to improve the efficiency of photon conversion (quantum dot solar cell), enable low-cost deposition of thin-films, provide sites for exciton dissociation, and pathways for electron transport. Quantum dots are also expected to be more resistant to degradation from electron, proton, and alpha particle radiation than the corresponding bulk material, a requirement for use in space solar ~sells. Chalcopyrite nanocrystals can be produced by low-temperature thermal decomposition of single-source precursors such as (PR3)2CuIn(ER')4 (R = Ph, R' = Et, E = S; R = R' = Ph, E = Se). Single-source precursors are molecules which contain all the necessary elements for synthesis of a desired material. Thermal decomposition of the precursor results in the formation of material with the correct stoichiometry as a nanocrystalline powder or a thin film, often at significantly lower temperatures than those typically employed for thin-film deposition by multi-source evaporation techniques, typically less than 500 C. We show that CuInSz and CuInSe2 nanocrystals can be synthesized from the precursors at temperatures as low as 250 C. The nanocrystals are characterized by optical spectroscopy, X-ray diffraction, and electron microscopy.

Castro, S. L.↗
NASA NTRS1999

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

Gas-phase combustion (flame) synthesis has been an essential industrial process for producing large quantities of powder materials such as carbon black, titanium dioxide, and silicon dioxide. Flames typically produce simple oxides, with carbon black being the noted exception because the oxides of carbon are gaseous and are easily separated from the particulate matter that is formed during fuel pyrolysis. Furthermore, the powders produced in flames are usually agglomerated, nanometer-sized particles (nanoparticles). This composition and morphology is acceptable for many applications. However, the present interest in nanoparticles for advanced materials application has led to efforts to employ flames for the synthesis of unagglomerated nanoparticles (2 to 100 nm) of metals and non-oxide ceramics. Sodium-halide chemistry has proven to be viable for producing metals and non-oxide ceramics in flames. Materials that have been produced to date include Si (Calcote and Felder, 1993), TiN, TiB2, TiC, TiSi2, SiC, B4C (Glassman et al, 1993) Al, W, Ti, TiB2, AlN, and W-Ti and Al-AlN composites (DuFaux and Axelbaum, 1995, Axelbaum et al 1996,1997). Many more materials are possible. The main challenge that faces application of flame synthesis for advanced materials is overcoming formation of agglomerates in flames (Brezinsky, 1997). The high temperatures and high number densities in the flame environment favor the formation of agglomerates. Agglomerates must be avoided for many reasons. For example, when nanopowders are consolidated, agglomerates have a deleterious effect on compaction density, leading to voids in the final part. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Another critical challenge that faces all synthesis routes for nanopowders is ensuring that the powders are high purity and that the process is scaleable. Though the containerless, high temperature environment of a flame is excellent for producing high-purity simple compounds, ultrafine metals and non-oxide ceramic powders are inherently reactive in the presence of oxygen and/or moisture. Thus, the handling of these powders after synthesis poses a challenging problem. Impurities acquired during handling of nanoparticles have plagued the advancement of nanostructured materials technology.

Sun, Z.↗
NASA NTRS2003

Carbon Nanotube Synthesis in a Flame with Independently Prepared Laser-Ablated Catalyst Particles

Laser ablation has been used ex situ to create metal nanoparticles for introduction into a reactive pyrolysis flame. By prior synthesis of the metal nanoparticles, the effects of the reactive gases can be clearly separated from the pyrolysis chemistry of a solvent carrier, as when nebulized solutions are used. Moreover, varying reactivity issues associated with particle growth and size are bypassed. Our results show that Fe selectively reacts with CO to produce nanotubes, whereas Ni selectively reacts with C2H2 to produce nanofibers. These observations are interpreted through the donation and withdrawal of electron density between the adsorbate's molecular orbitals and surface atoms of the metal nanoparticle. The rate of reaction of Ni with only C2H2 is found to be greater than the rate with C2H2 and CO. This suggests that CO inhibits the Ni-catalyzed reaction.

Nanotubes, Carbon/chemistry/ultrastructure↗
NASA NTRS2003

Synthesis of substantially monodispersed colloids

A method of forming ligated nanoparticles of the formula Y(Z).sub.x where Y is a nanoparticle selected from the group consisting of elemental metals having atomic numbers ranging from 21-34, 39-52, 57-83 and 89-102, all inclusive, the halides, oxides and sulfides of such metals, and the alkali metal and alkaline earth metal halides, and Z represents ligand moieties such as the alkyl thiols. In the method, a first colloidal dispersion is formed made up of nanoparticles solvated in a molar excess of a first solvent (preferably a ketone such as acetone), a second solvent different than the first solvent (preferably an organic aryl solvent such as toluene) and a quantity of ligand moieties; the first solvent is then removed under vacuum and the ligand moieties ligate to the nanoparticles to give a second colloidal dispersion of the ligated nanoparticles solvated in the second solvent. If substantially monodispersed nanoparticles are desired, the second dispersion is subjected to a digestive ripening process. Upon drying, the ligated nanoparticles may form a three-dimensional superlattice structure.

Klabunde, Kenneth J.↗