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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 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1990

Studies on the use of supercritical ammonia for ceramic nitride synthesis and fabrication

The extractability of ammonia halides (including ammonium thiocyanate) formed as byproducts from the synthesis of Si(NH)2 via ammonolysis of the corresponding silicon tetrahalides using supercritical NH3 as the extraction medium was investigated. It was found that the NH4SCN byproduct of ammonolysis of Si(SCN)4 can be almost completely extracted from the insoluble Si(NH)2 forming a promising system for the synthesis of pure Si(NH)2, one of the best precursors for Si3N4. In addition it was found that Si3N4, AlN, BN, and Si(NH)2 are insoluble in SC ammonia. Also discussed are design considerations for a supercritical ammonia extraction unit.

Cornell, Linda↗
NASA NTRS2014

Boron Nitride Nanotube: Synthesis and Applications

Scientists have predicted that carbon's immediate neighbors on the periodic chart, boron and nitrogen, may also form perfect nanotubes, since the advent of carbon nanotubes (CNTs) in 1991. First proposed then synthesized by researchers at UC Berkeley in the mid 1990's, the boron nitride nanotube (BNNT) has proven very difficult to make until now. Herein we provide an update on a catalyst-free method for synthesizing highly crystalline, small diameter BNNTs with a high aspect ratio using a high power laser under a high pressure and high temperature environment first discovered jointly by NASA/NIA JSA. Progress in purification methods, dispersion studies, BNNT mat and composite formation, and modeling and diagnostics will also be presented. The white BNNTs offer extraordinary properties including neutron radiation shielding, piezoelectricity, thermal oxidative stability (> 800 C in air), mechanical strength, and toughness. The characteristics of the novel BNNTs and BNNT polymer composites and their potential applications are discussed.

Tiano, Amanda L.↗
NASA NTRS1993

Synthesis, Properties, and Applications Of Boron Nitride

Report describes synthesis, properties, and applications of boron nitride. Especially in thin-film form. Boron nitride films useful as masks in x-ray lithography; as layers for passivation of high-speed microelectronic circuits; insulating films; hard, wear-resistant, protective films for optical components; lubricants; and radiation detectors. Present status of single-crystal growth of boron nitride indicates promising candidate for use in high-temperature semiconductor electronics.

Pouch, John J.↗
NASA NTRS1996

Gas-Phase Combustion Synthesis of Aluminum Nitride Powder

Due to its combined properties of high electrical resistivity and high thermal conductivity aluminum nitride (AlN) is a highly desirable material for electronics applications. Methods are being sought for synthesis of unagglomerated, nanometer-sized powders of this material, prepared in such a way that they can be consolidated into solid compacts having minimal oxygen content. A procedure for synthesizing these powders through gas-phase combustion is described. This novel approach involves reacting AlCl3, NH3, and Na vapors. Equilibrium thermodynamic calculations show that 100% yields can be obtained for these reactants with the products being AlN, NaCl, and H2. The NaCl by-product is used to coat the AlN particles in situ. The coating allows for control of AlN agglomeration and protects the powders from hydrolysis during post-flame handling. On the basis of thermodynamic and kinetic considerations, two different approaches were employed to produce the powder, in co-flow diffusion flame configurations. In the first approach, the three reactants were supplied in separate streams. In the second, the AlCl3 and NH3 were premixed with HCl and then reacted with Na vapor. X-ray diffraction (XRD) spectra of as-produced powders show only NaCl for the first case and NaCl and AlN for the second. After annealing at 775 C tinder dynamic vacuum, the salt was removed and XRD spectra of powders from both approaches show only AlN. Aluminum metal was also produced in the co-flow flame by reacting AlCl3 with Na. XRD spectra of as-produced powders show the products to be only NaCl and elemental aluminum.

Axelbaum, R. L.↗
NASA NTRS2005

Synthesis of Boron Nitride Nanotubes for Engineering Applications

Boron Nitride nanotubes (BNNT) are of interest to the scientific and technical communities for many of the same reasons that carbon nanotubes (CNT) have attracted large amounts of attention. Both materials have potentially unique and significant properties which may have important structural and electronic applications in the future. However of even more interest than their similarities may be the differences between carbon and boron nanotubes. Whilt boron nitride nanotubes possess a very high modulus similaar to CNT, they are also more chemically and thermally inert. Additionally BNNT possess more uniform electronic properties, having a uniform band gap of approximately 5.5 eV while CNT vary from semi-conductin to conductor behavior. Boron Nitride nanotubes have been synthesized by a variety of methods such as chemical vapor deposition, arc discharge and reactive milling. Consistently producing a reliable product has proven difficult. Progress in synthesis of 1-2 gram sized batches of Boron Nitride nanotubes will be discussed as well as potential uses for this unique material.

Hurst, Janet↗
NASA NTRS2016

Radio Frequency Plasma Synthesis of Boron Nitride Nanotubes (BNNTs) for Structural Applications: Part I

It is evident that nanotubes, such as carbon, boron nitride and even silicon, offer great potential for many aerospace applications. The opportunity exists to harness the extremely high strength and stiffness exhibited by high-purity, low-defect nanotubes in structural materials. Even though the technology associated with carbon nanotube (CNT) development is mature, the mechanical property benefits have yet to be fully realized. Boron nitride nanotubes (BNNTs) offer similar structural benefits, but exhibit superior chemical and thermal stability. A broader range of potential structural applications results, particularly as reinforcing agents for metal- and ceramic- based composites. However, synthesis of BNNTs is more challenging than CNTs mainly because of the higher processing temperatures required, and mass production techniques have yet to emerge. A promising technique is radio frequency plasma spray (RFPS), which is an inductively coupled, very high temperature process. The lack of electrodes and the self- contained, inert gas environment lend themselves to an ultraclean product. It is the aim of this White Paper to survey the state of the art with regard to nano-material production by analyzing the pros and cons of existing methods. The intention is to combine the best concepts and apply the NASA Langley Research Center (LaRC) RFPS facility to reliably synthesize large quantities of consistent, high-purity BNNTs.

Hales, Stephen J.↗
NASA NTRS2021

Radio Frequency Plasma Synthesis of Boron Nitride Nanotubes (BNNTs) for Structural Applications: Part III

The emergence of commercial quantities of BNNTs facilitates the exploration of structural material applications. BNNT-reinforced composites must exhibit extraordinary mechanical properties in order to justify the cost premium. Prevailing theory indicates that suitable BNNTs must possess an aspect ratio (AR= length/diameter) approaching 10,000 to provide effective discontinuous reinforcement under tensile loading. A survey of commercial products shows that although the quantities are sufficient, lots of uniform morphology are unavailable. Therefore, the opportunity exists to supplement procedures either during synthesis operations or post-synthesis processing in order to deliver homogeneous batches of high AR BNNTs. An assessment of relevant technologies reveals established methods compatible with sorting of BNNTs by physical dimensions, i.e., size and/or shape. Electrostatic fractionation emerges as the leading candidate, with the potential to isolate high-purity, low-defect, high AR product. The adaptation of existing equipment to the handling of fibrous particulate on the nanoscale will be paramount to success. Although currently focused on BNNTs, the concepts outlined may be applied to nanotubes synthesized from any organic or inorganic compounds. This survey sets the stage for delivering reproducible lots of BNNTs that satisfy the dimensional requirements for use in acreage structural materials.

induction plasma, BNNT, aspect ratio, fractionatio↗
NASA NTRS2016

Radio Frequency Plasma Synthesis of Boron Nitride Nanotubes (BNNTs) for Structural Applications

Boron nitride nanotubes (BNNTs) are more thermally and chemically compatible with metal- and ceramic-matrix composites than carbon nanotubes (CNTs). The lack of an abundant supply of defect-free, high-aspect-ratio BNNTs has hindered development as reinforcing agents in structural materials. Recent activities at the National Research Council - Canada (NRC-C) and the University of California - Berkeley (UC-B) have resulted in bulk synthesis of few-walled, small diameter BNNTs. Both processes employ induction plasma technology to create boron vapor and highly reactive nitrogen species at temperatures in excess of 8000 K. Subsequent recombination under controlled cooling conditions results in the formation of BNNTs at a rate of 20 g/hr and 35 g/hr, respectively. The end product tends to consist of tangled masses of fibril-, sheet-, and cotton candy-like materials, which accumulate within the processing equipment. The radio frequency plasma spray (RFPS) facility at NASA Langley (LaRC), developed for metallic materials deposition, has been re-tooled for in-situ synthesis of BNNTs. The NRC-C and UC-B facilities comprise a 60 kW RF torch, a reactor with a stove pipe geometry, and a filtration system. In contrast, the LaRC facility has a 100 kW torch mounted atop an expansive reaction chamber coupled with a cyclone separator. The intent is to take advantage of both the extra power and the equipment configuration to simultaneously produce and gather BNNTs in a macroscopic form amenable to structural material applications.

Hales, Stephen J.↗
NASA NTRS2014

High-Speed Imaging Optical Pyrometry for Study of Boron Nitride Nanotube Generation

A high-speed imaging optical pyrometry system is designed for making in-situ measurements of boron temperature during the boron nitride nanotube synthesis process. Spectrometer measurements show molten boron emission to be essentially graybody in nature, lacking spectral emission fine structure over the visible range of the electromagnetic spectrum. Camera calibration experiments are performed and compared with theoretical calculations to quantitatively establish the relationship between observed signal intensity and temperature. The one-color pyrometry technique described herein involves measuring temperature based upon the absolute signal intensity observed through a narrowband spectral filter, while the two-color technique uses the ratio of the signals through two spectrally separated filters. The present study calibrated both the one- and two-color techniques at temperatures between 1,173 K and 1,591 K using a pco.dimax HD CMOS-based camera along with three such filters having transmission peaks near 550 nm, 632.8 nm, and 800 nm.

Inman, Jennifer A.↗
NASA NTRS2019

Exceptional Thermal Properties of Polymer-Derived Ceramic Composites Reinforced with High Volume Fractions of Boron Nitride Nanotube at Elevated Temperature

We report for the first time the synthesis of boron nitride nanotube (BNNT) reinforced ceramic composites using the polymer derived ceramic (PDC) processing route. The nanocomposites had a BNNT loading of up to 35.4 vol.%. TGA results showed that the nanocomposites have good thermal stability up to 900 oC in air. BNNTs in the nanocomposites survived in an oxidizing environment up to 900 oC, revealing that the nanocomposites can be used for high temperature applications. Thermal conductivity of PDC reinforced with 35.4 vol.% BNNT was measured as 4.123 W/(m·K) at room temperature, which is a 2100 % increase compared to that of pristine PDC. The thermal conductivity value increases with the increase of BNNT content. A thermal conductivity percolation phenomenon appeared when the BNNT content increased to 36±5 vol.%. The results of this study showed that BNNTs could effectively improve the thermal conductivity of PDC materials. BNNT reinforced PDC could be used as thermal structural materials in a harsh environment at the temperature up to 900 deg C.

Yujun Jia↗
NASA NTRS1994

Synthesis Of A Precursor Of Silicon Nitride

Promising route toward production of highly pure, finely divided, easily sinterable silicon nitride (Si3N4) involves thermal decomposition of silicon diimide {Si(NH)2} prepared by ammonolysis of Si(SCN)4 in CH3CN and purified by complete extraction of byproduct NH4SCN by use of ammonia at temperature and pressure above critical point.

Philipp, Warren H.↗
NASA NTRSDate not supplied

Forcespun Polymers as Precursors to Boron Nitride Fibers

The need for multifunctional materials in aerospace technologies is currently driving the development of new novel composite materials. Specifically, insulation materials with high thermal conductivity, high electrical resistivity, and are chemically inert are needed for high voltage power applications. Boron nitride (BN) nanomaterials fit these criteria and can be incorporated into composites for further material design. The synthesis of boron nitride through a polymer derived ceramic route allows for the morphology of the resulting BN to be tailored. This is especially beneficial since the polymers can be shaped or spun into fibers prior to the ceramic conversion. This project utilizes the Forcespinning technique to produce boron-containing polymer fibers that are converted to boron nitride through a heat treatment. The chemical compositions and fiber morphologies were studied and reported here.

Boron nitride, Fibers, Forcespinning↗
NASA NTRS1983

Synthesis of N-Substituted Silaneamines: Monomeric Precursors of Silicon Carbide-Nitride Fibers

Silanetriamines are prepared by the condensation of methyl or phenyl trichlorosilane with a primary amine. The amines used were methyl, n-propyl, n-butyl and allyl. The silaneamines were prepared by adding the chlorosilane to a solution of the amine in either petroleum ether or toluene. The compounds were purified by distillation and characterized by infrared and nuclear magnetic resonance spectroscopy.

Crouse, D. J.↗
NASA NTRS1980

Hot isostatic pressing of silicon nitride Sisub3n4 containing zircon, or zirconia and silica

A hydrothermal synthesis apparatus with a 10 KB cylinder was used to obtain a sintered body of silicon nitride. The sintering auxiliary agents used were zircon (ZrSiO4) and a mixture of zirconia (ZrO2) and silica (SiO2). Experiments were conducted with the amounts of ZrSi04 or ArO2 and SiO2 varying over a wide range and the results compared to discover the quantity of additive which produced sintering in silicon nitride by the hot pressing method.

Somiya, S.↗
NASA NTRS1988

Comparison of the surface charge behavior of commercial silicon nitride and silicon carbide powders

The adsorption and desorption of protons from aqueous solution onto the surfaces of a variety of commercial silicon carbide and silicon nitride powders has been examined using a surface titration methodology. This method provides information on some colloidal characteristics, such as the point of zero charge (pzc) and the variation of proton adsorption with dispersion pH, useful for the prediction of optimal ceramic-processing conditions. Qualitatively, the magnitude of the proton adsorption from solution reveals small differences among all of the materials studied. However, the results show that the pzc for the various silicon nitride powders is affected by the powder synthesis route. Complementary investigations have shown that milling can also act to shift the pzc exhibited by silicon nitride powder. Also, studies of the role of the electrolyte in the development of surface charge have indicated no evidence of specific adsorption of ammonium ion on either silicon nitride or silicon carbide powders.

Whitman, Pamela K.↗
NASA NTRS2005

Boron Nitride Nanotubes for Engineering Applications

Boron nitride nanotubes (BNNT) are of significant interest to the scientific and technical communities for many of the same reasons that carbon nanotubes (CNT) have attracted wide attention. Both materials have potentially unique and important properties for structural and electronic applications. However of even more consequence than their similarities may be the complementary differences between carbon and boron nitride nanotubes While BNNT possess a very high modulus similar to CNT, they also possess superior chemical and thermal stability. Additionally, BNNT have more uniform electronic properties, with a uniform band gap of 5.5 eV while CNT vary from semi-conductive to highly conductive behavior. Boron nitride nanotubes have been synthesized both in the literature and at NASA Glenn Research Center, by a variety of methods such as chemical vapor deposition, arc discharge and reactive milling. Consistent large scale production of a reliable product has proven difficult. Progress in the reproducible synthesis of 1-2 gram sized batches of boron nitride nanotubes will be discussed as well as potential uses for this unique material.

Hurst, Janet↗
NASA NTRS1987

Stability and rheology of dispersions of silicon nitride and silicon carbide

The relationship between the surface and colloid chemistry of commercial ultra-fine silicon carbide and silicon nitride powders was examined by a variety of standard characterization techniques and by methodologies especially developed for ceramic dispersions. These include electrokinetic measurement, surface titration, and surface spectroscopies. The effects of powder pretreatment and modification strategies, which can be utilized to augment control of processing characteristics, were monitored with these technologies. Both silicon carbide and nitride were found to exhibit silica-like surface chemistries, but silicon nitride powders possess an additional amine surface functionality. Colloidal characteristics of the various nitride powders in aqueous suspension is believed to be highly dependent on the relative amounts of the two types of surface groups, which in turn is determined by the powder synthesis route. The differences in the apparent colloidal characteristics for silicon nitride powders cannot be attributed to the specific absorption of ammonium ions. Development of a model for the prediction of double-layer characteristics of materials with a hybrid site interface facilitated understanding and prediction of the behavior of both surface charge and surface potential for these materials. The utility of the model in application to silicon nitride powders was demonstrated.

Feke, Donald L.↗