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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 NTRS1993

Tool grinding and spark testing

The objectives were the following: (1) to revive the neglected art of metal-sparking; (2) to promote quality-assurance in the workplace; (3) to avoid spark-ignited explosions of dusts or volatiles; (4) to facilitate the salvage of scrap metals; and (5) to summarize important references.

Widener, Edward L.↗

NASA NTRS2010

Promoted Combustion Test Data Re-Examined

Promoted combustion testing of metallic materials has been performed by NASA since the mid-1980s to determine the burn resistance of materials in oxygen-enriched environments. As the technolo gy has advanced, the method of interpreting, presenting, and applying the promoted combustion data has advanced as well. Recently NASA changed the bum criterion from 15 cm (6 in.) to 3 cm (1.2 in.). This new burn criterion was adopted for ASTM G 124, Standard Test Method for Determining the Combustion Behavior- of Metallic Materials in Oxygen-Enriched Atmospheres. Its effect on the test data and the latest method to display the test data will be discussed. Two specific examples that illustrate how this new criterion affects the burn/no-bum thresholds of metal alloys will also be presented.

Lewis, Michelle↗

NASA NTRS2009

Method of Suppressing Sublimation in Advanced Thermoelectric Devices

A method of applying a physical barrier to suppress thermal decomposition near a surface of a thermoelectric material including applying a continuous metal foil to a predetermined portion of the surface of the thermoelectric material, physically binding the continuous metal foil to the surface of the thermoelectric material using a binding member, and heating in a predetermined atmosphere the applied and physically bound continuous metal foil and the thermoelectric material to a sufficient temperature in order to promote bonding between the continuous metal foil and the surface of the thermoelectric material. The continuous metal foil forms a physical barrier to enclose a predetermined portion of the surface. Thermal decomposition is suppressed at the surface of the thermoelectric material enclosed by the physical barrier when the thermoelectric element is in operation.

Sakamoto, Jeffrey S.↗

NASA NTRS2006

Promoted-Combustion Chamber with Induction Heating Coil

An improved promoted-combustion system has been developed for studying the effects of elevated temperatures on the flammability of metals in pure oxygen. In prior promoted-combustion chambers, initial temperatures of metal specimens in experiments have been limited to the temperatures of gas supplies, usually near room temperature. Although limited elevated temperature promoted-combustion chambers have been developed using water-cooled induction coils for preheating specimens, these designs have been limited to low-pressure operation due to the hollow induction coil. In contrast, the improved promoted-combustion chamber can sustain a pressure up to 10 kpsi (69 MPa) and, through utilization of a solid induction coil, is capable of preheating a metal specimen up to its melting point [potentially in excess of 2,000 F (approximately equal to 1,100 C)]. Hence, the improved promoted combustion chamber makes a greater range of physical conditions and material properties accessible for experimentation. The chamber consists of a vertical cylindrical housing with an inner diameter of 8 in. (20.32 cm) and an inner height of 20.4 in. (51.81 cm). A threaded, sealing cover at one end of the housing can be unscrewed to gain access for installing a specimen. Inlet and outlet ports for gases are provided. Six openings arranged in a helical pattern in the chamber wall contain sealed sapphire windows for viewing an experiment in progress. The base of the chamber contains pressure-sealed electrical connectors for supplying power to the induction coil. The connectors feature a unique design that prevents induction heating of the housing and the pressure sealing surfaces; this is important because if such spurious induction heating were allowed to occur, chamber pressure could be lost. The induction coil is 10 in. (25.4 cm) long and is fitted with a specimen holder at its upper end. At its lower end, the induction coil is mounted on a ceramic base, which affords thermal insulation to prevent heating of the base of the chamber during use. A sapphire cylinder protects the coil against slag generated during an experiment. The induction coil is energized by a 6-kW water-cooled power supply operating at a frequency of 400 kHz. The induction coil is part of a parallel-tuned circuit, the tuning of which is used to adjust the coupling of power to the specimen. The chamber is mounted on a test stand along with pumps, valves, and plumbing for transferring pressurized gas into and out of the chamber. In addition to multiple video cameras aimed through the windows encircling the chamber, the chamber is instrumented with gauges for monitoring the progress of an experiment. One of the gauges is a dual-frequency infrared temperature transducer aimed at the specimen through one window. Chamber operation is achieved via a console that contains a computer running apparatus-specific software, a video recorder, and real-time video monitors. For safety, a blast wall separates the console from the test stand.

Richardson, Erin↗

NASA NTRS2000

Test System to Study the Ignition of Metals by Polymers in Oxygen

A new test system that uses Laser energy to ignite a polymer promoter has been developed at the NASA White Sands Test Facility. It will facilitate the study of the spread of fire from a burning polymer material to the metal surrounding it. The system can be used to answer questions regarding the effects of configuration on ignition and combustion. The data obtained from this test could also be used to develop mathematical models for analyzing the effects of configuration on ignition and combustion. The system features a 10,000-psi (69-MPa) test chamber with sight glass windows on either end and a 25-watt carbon dioxide Laser for an ignition source. The test system can be used with gaseous oxygen, nitrogen or any mixture of the two gases. To minimize the effect of preheating the metallic, the polymer is ignited with a minimal amount of Laser energy. Igniting the polymer in this fashion also simplifies the thermodynamic analysis of the ignition and propagation reactions. The system is very robust, versatile and straightforward to use. Depending on the test pressure and configuration, the test system operator can perform as many as 20 tests per day. Test results verify that ignition and combustion of the metallic sample is not only dependent on pressure, material type and temperature, but configuration of both the polymer promoter and metallic sample. Both 6061 aluminum and 316 stainless steel 0.25-inch (6.35-mm) diameter rods with a standard 0-ring groove were tested with Buna-N, Silicone, Teflon and Viton 0-rings. The system ignited all four types of 0-rings in oxygen at pressures ranging from ambient to 10,000 psi (69 MPa). However, neither the stainless steel nor the aluminum rods on which the O-rings were mounted ignited in any test conditions. Future testing may be done on the 0.25-inch (6.35-mm) rod and O-ring configuration to evaluate the lack of ignition in these tests. Future configurations may include a plug of polymer in the base of the sample and replicas of fire-damaged components. Furthermore, the test system may be used in the future to analyze the oxidation rate of Laser-heated metals in gaseous oxygen.

Shoffstall, Michael S.↗

NASA NTRS2010

Heat Effects of Promoters and Determination of Burn Criterion in Promoted Combustion Testing

Promoted ignition testing (NASA Test 17) [1] is used to determine the relative flammability of metal rods in oxygen-enriched atmospheres. A promoter is used to ignite a metal sample rod, initiating sample burning. If a predetermined length of the sample burns, beyond the promoter, the material is considered flammable at the condition tested. Historically, this burn length has been somewhat arbitrary. Experiments were performed to better understand this test by obtaining insight into the effect a burning promoter has on the preheating of a test sample. Test samples of several metallic materials were prepared and coupled to fast-responding thermocouples along their length. Thermocouple measurements and test video were synchronized to determine temperature increase with respect to time and length along each test sample. A recommended flammability burn length, based on a sample preheat of 500 F, was determined based on the preheated zone measured from these tests. This length was determined to be 30 mm (1.18 in.). Validation of this length and its rationale are presented.

Sparks, Kyle M.↗

NASA NTRS2009

Determination of Pass/Fail Criteria for Promoted Combustion Testing

Promoted ignition testing is used to determine the relative flammability of metal rods in oxygen-enriched atmospheres. In these tests, a promoter is used to ignite each metal rod to start the sample burning. Experiments were performed to better understand the promoted ignition test by obtaining insight into the effect a burning promoter has on the preheating of a test sample. Test samples of several metallic materials were prepared and coupled to fast-responding thermocouples along their length. Various ignition promoters were used to ignite the test samples. The thermocouple measurements and test video was synchronized to determine temperature increase with respect to time and length along each test sample. A recommended length of test sample that must be consumed to be considered a flammable material was determined based on the preheated zone measured from these tests. This length was determined to be 30 mm (1.18 in.). Validation of this length and its rationale are presented.

Sparks, Kyle M.↗

NASA NTRS1989

Flammability and sensitivity of materials in oxygen-enriched atmospheres; Proceedings of the Fourth International Symposium, Las Cruces, NM, Apr. 11-13, 1989. Volume 4

The present volume discusses the ignition of nonmetallic materials by the impact of high-pressure oxygen, the promoted combustion of nine structural metals in high-pressure gaseous oxygen, the oxygen sensitivity/compatibility ranking of several materials by different test methods, the ignition behavior of silicon greases in oxygen atmospheres, fire spread rates along cylindrical metal rods in high-pressure oxygen, and the design of an ignition-resistant, high pressure/temperature oxygen valve. Also discussed are the promoted ignition of oxygen regulators, the ignition of PTFE-lined flexible hoses by rapid pressurization with oxygen, evolving nonswelling elastomers for high-pressure oxygen environments, the evaluation of systems for oxygen service through the use of the quantitative fault-tree analysis, and oxygen-enriched fires during surgery of the head and neck.

Stoltzfus, Joel M.↗

NASA NTRS1993

Influence of test configuration on the combustion characteristics of polymers as ignition sources

The experimental evaluation of polymers as ignition sources for metals was accomplished at the NASA White Sands Test Facility (WSTF) using a standard promoted combustion test. These tests involve the transient burning of materials in high-pressure oxygen environments. They have provided data from which design decisions can be made; data include video recordings of ignition and non-ignition for specific combinations of metals and polymers. Other tests provide the measured compositions of combustion products for polymers at select burn times and an empirical basis for estimating burn rates. With the current test configuration, the detailed analysis of test results requires modeling a three-dimensional, transient convection process involving fluid motion, thermal conduction and convection, the diffusion of chemical species, and the erosion of sample surface. At the high pressure extremes, it even requires the analysis of turbulent, transient convection where the physics of the problem are not well known and the computation requirements are not practical at this time. An alternative test configuration that can be analyzed with a relatively-simple convection model was developed during the summer period. The principal change constitutes replacing a large-diameter polymer disk at the end of the metal test rod with coaxial polymer cylinders that have a diameter nearer to that of the metal rod. The experimental objective is to assess the importance of test geometries on the promotion of metal ignition by testing with different lengths of the polymer and, with an extended effort, to analyze the surface combustion in the redesigned promoted combustion tests through analytical modeling of the process. The analysis shall use the results of cone-calorimeter tests of the polymer material to model primary chemical reactions and, with proper design of the promoted combustion test, modeling of the convection process could be conveniently limited to a quasi-steady boundary layer analysis where the economical solution of parabolic equations is involved. The products for the summer period are: (1) a conceptual-level redesign of the test apparatus, and (2) the development and use of an approximate integral boundary layer analysis to demonstrate the influence of geometry changes prior to testing. A computer code STAN5, an accurate numerical boundary layer model whose earlier versions were developed for the NASA Lewis Research Center by the Fellow, also was installed and validated on the WSTF and New Mexico State University computer systems as a starting point in the development of a more detailed fluid mechanics and combustion model.

Julien, Howard L.↗

NASA NTRS1990

Comparison of the bonding between ML(+) and ML2(+) (M = metal, L = noble gas)

Ab initio calculations are reported of the spectroscopic constants for the low-lying states of the molecular ions ML2(+), where M = Li, Na, Mg, V, Fe, Co, Ni and Cu, and where L is usually Ar. Comparison with existing analogous calculations on the ML(+) ions shows how the bonding and binding energy change with the addition of a second noble gas atom. The second binding energy is predicted to be essentially the same as the first for the Li, Na, Mg, and V ions, but larger for the Fe, Co, Ni and Cu ions. The binding energies of the transition metal noble gas ions are not accurately predicted at the SCF level, because correlation is required to describe their M(0)Ln(+) character. All trends can be explained in terms of promotion and hybridization on the metal ion.

Bauschlicher, Charles W., Jr.↗

NASA NTRS1974

Dissimilar metals joint evaluation

Dissimilar metals tubular joints between 2219-T851 aluminum alloy and 304L stainless steel were fabricated and tested to evaluate bonding processes. Joints were fabricated by four processes: (1) inertia (friction) weldings, where the metals are spun and forced together to create the weld; (2) explosive welding, where the metals are impacted together at high velocity; (3) co-extrusion, where the metals are extruded in contact at high temperature to promote diffusion; and (4) swaging, where residual stresses in the metals after a stretching operation maintain forced contact in mutual shear areas. Fifteen joints of each type were prepared and evaluated in a 6.35 cm (2.50 in.) O.D. size, with 0.32 cm (0.13 in.) wall thickness, and 7.6 cm (3.0 in) total length. The joints were tested to evaluate their ability to withstand pressure cycle, thermal cycle, galvanic corrosion and burst tests. Leakage tests and other non-destructive test techniques were used to evaluate the behavior of the joints, and the microstructure of the bond areas was analyzed.

Wakefield, M. E.↗

NASA NTRS1988

ASTM Committee G-4 metals flammability test program - Data and discussion

Results of metals flammability tests performed on twenty-six metals in the NASA/White Sands Test Facility are discussed together with the test systems. The promoted combustion and ignition characteristics of these metals are described, and the metals are ranked according to their suitability for use in oxygen systems. In general, alloys with high copper and nickel contents and low iron content were found to rank higher than those that had high iron content, while alloys that had high aluminum content were ranked the lowest.

Stoltzfus, Joel M.↗

NASA NTRS1983

Studies of the mechanisms of turbine fuel instability

The formation of insoluble deposits in a Jet A, a Diesel, and a model fuel (1/10 v/v tetralin/dodecane) was studied. Experiments were conducted using glass containers at 394 K with an air/fuel ratio of 14/1. The effects of addition of ppm levels of various compounds on deposit formation were evaluated. Nitrogen heterocycles were shown to produce a basicity dependent acceleration of deposition. Thiols and thiophene were shown to increase deposition while sulfides and disulfides act as inhibitors. Copper metal and its salts also promote deposition. Results of various instrumental analyses of deposits and development of a high performance liquid chromatographic method for monitoring deposit precursors are discussed.

Daniel, S. R.↗

NASA NTRS1993

XPS analysis of the effect of fillers on PTFE transfer film development in sliding contacts

The development of transfer films atop steel counterfaces in contact with unfilled and bronze-filled PTFE has been studied using X-ray photoelectron spectroscopy. The sliding apparatus was contained within the vacuum of the analytical system, so the effects of the native oxide, hydrocarbon, and adsorbed gaseous surface layers of the steel upon the PTFE transfer behavior could be studied in situ. For both the filled and the unfilled PTFE, cleaner surfaces promoted greater amounts of transfer. Metal fluorides, which formed at the transfer film/counterface interface, were found solely in cases where the native oxide had been removed to expose the metallic surface prior to sliding. These fluorides also were found at clean metal/PTFE interfaces formed in the absence of frictional contact. A fraction of these fluorides resulted from irradiation damage inherent in XPS analysis. PTFE transfer films were found to build up with repeated sliding passes, by a process in which strands of transfer filled in the remaining counterface area. Under these reported test conditions, the transfer process is not expected to continue atop previously deposited transfer films. The bronze-filled composite generated greater amounts of transfer than the unfilled PTFE. The results are discussed relative to the observed increase in wear resistance imparted to PTFE by a broad range of inorganic fillers.

Blanchet, T. A.↗

NASA NTRS1995

The Study of the Successive Metal-Ligand Binding Energies for Fe(sup +), Fe(sup -), V(sup +) and Co(sup +)

The successive binding energies of CO and H2O to Fe(sup +), CO to Fe(sup -), and H2 to Co(sup +) and V(sup +) are presented. Overall the computed results are in good agreement with experiment. The trends in binding energies are analyzed in terms of metal to ligand donation, ligand to metal donation, ligand-ligand repulsion, and changes in the metal atom, such as hybridization, promotion, and spin multiplicity. The geometry and vibrational frequencies are also shown to be directly affected by these effects.

Bauschlicher, Charles W., Jr.↗

NASA NTRS1994

The Study of the Successive Metal-ligand Binding Energies for Fe(+), Fe(-), V(+) and Co(+)

The successive binding energies of CO and H2O to Fe(+), CO to Fe(-), and H2 to Co(+) and V(+) are presented. Overall the computed results are in good agreement with experiment. The trends in binding energies are analyzed in terms of metal to ligand donation, ligand to metal donation, ligand-ligand repulsion, and changes in the metal atom, such as hybridization, promotion, and spin multiplicity. The geometry and vibrational frequencies are also shown to be directly affected by these effects.

Bauschlicher, Charles W., Jr.↗

NASA NTRS1995

The Study Of The Successive Metal-Ligand Binding Energies For Fe+, Fe-, V+ and Co+

Bauschicher, Charles W., Jr.↗