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NASA NTRS2004

Epoxy Adhesives for Stator Magnet Assembly in Stirling Radioisotope Generators (SRG)

As NASA seeks to fulfill its goals of exploration and understanding through missions planned to visit the moons of Saturn and beyond, a number of challenges arise from the idea of deep space flight. One of the first problems associated with deep space travel is electrical power production for systems on the spacecraft. Conventional methods such as solar power are not practical because efficiency decreases substantially as the craft moves away from the Sun. The criterion for power generation during deep space missions are very specific, the main points requiring high reliability, low mass, minimal vibration and a long lifespan. A Stirling generator, although fairly old in concept, is considered to be a potential solution for electrical power generation for deep space flight. A Stirling generator works on the same electromagnetic principles of a standard generator, using the linear motion of the alternator through the stationary stator which produces electric induction. The motion of the alternator, however, is produced by the heating and cooling dynamics of pressurized gases. Essentially heating one end and cooling another of a contained gas will cause a periodic expansion and compression of the gas from one side to the other, which a displacer translates into linear mechanical motion. NASA needs to confirm that the materials used in the generator will be able to withstand the rigors of space and the life expectancy of the mission. I am working on the verification of the epoxy adhesives used to bond magnets to the steel lamination stack to complete the stator; in terms of in-service performance and durability under various space environments. Understanding the proper curing conditions, high temperature properties, and degassing problems as well as production difficulties are crucial to the long term success of the generator. system and steel substrate used in the stator. To optimize the curing conditions of the epoxies, modulated differential scanning calorimetry analysis was done as a function of cure time and temperatures. Adhesion bond strength was tested at various temperatures with lap shear samples using Hiperco 50 substrate to ensure that the proper adhesive is being used. To try and solve the problem of bondline thickness, micro glass beads of 0.0017" in diameter were investigated to see if any other physical properties of the epoxy were affected. Efforts will be made to develop a standard, optimized, fabrication process/procedure of sub-scale magnet-stator assemblies for various adhesive performance evaluation studies under simulated generator conditions. Also, accelerated aging testing will be done in a pressurized canister with stator assembly samples for three years to verify if any degassing or thermal degradation of the epoxy occurs. The necessity of verifying the correct epoxy adhesive system for the stator magnet in the SRG is crucial because failure of the stator assembly would jeopardize the electrical system, and thereby the entire mission itself. My work involves specimen fabrications, testing, and data analyses of the epoxy adhesive system for the stator magnet in the SRG is crucial because failure of the stator assembly would jeopardize the electrical system, and thereby the entire mission itself.

Cater, George M.↗
NASA NTRS1988

A 1050 K Stirling space engine design

As part of the NASA CSTI High Capacity Power Program on Conversion Systems for Nuclear Applications, Sunpower, Inc. completed for NASA Lewis a reference design of a single-cylinder free-piston Stirling engine that is optimized for the lifetimes and temperatures appropriate for space applications. The NASA effort is part of the overall SP-100 program which is a combined DOD/DOE/NASA project to develop nuclear power for space. Stirling engines have been identified as a growth option for SP-100 offering increased power output and lower system mass and radiator area. Superalloy materials are used in the 1050 K hot end of the engine; the engine temperature ratio is 2.0. The engine design features simplified heat exchangers with heat input by sodium heat pipes, hydrodynamic gas bearings, a permanent magnet linear alternator, and a dynamic balance system. The design shows an efficiency (including the alternator) of 29 percent and a specific mass of 5.7 kg/kW. This design also represents a significant step toward the 1300 K refractory Stirling engine which is another growth option of SP-100.

Penswick, L. Barry↗
NASA NTRS2004

Time-Temperature Dependent Response of Filament Wound Composites for Flywheel Rotors

Flywheel energy storage offers an attractive alternative to battery systems used in space applications such as the International Space Station. Rotor designs capable of high specific energies benefit from the load carrying capacity of hoop wound carbon fibers but their long-term durability may be limited by time-temperature dependent radial deformations. This was investigated for the carbon/epoxy rotor material, IM7/8552. Coupon specimens were sectioned from filament wound panels. These were tested in compression and tension at room temperature (RT), 95 and 135 C for strain rates from 5x10(exp -6) per second to 5x10(exp -3) per second. Time, temperature and load sign dependent effects were significant transverse to the fiber. At -0.5 percent strain for 72 hr, compressive stresses relaxed 16.4 percent at 135 C and 13 percent at 95 C. Tensile stresses relaxed only 7 percent in 72 hr at 135 C for 0.5 percent strain. Using linear hereditary material response and Boltzmann s principle of superposition to describe this behavior is problematic if not intractable. Micromechanics analysis including the effects of processing residual stresses is needed to resolve the paradoxes. Uniaxial compressive stress relaxation data may be used to bound the loss of radial pre-load stresses in flywheel rotors.

Thesken, John C.↗
NASA NTRS2005

Supporting Development for the Stirling Radioisotope Generator and Advanced Stirling Technology Development at NASA Glenn Research Center

A high-efficiency, 110-We (watts electric) Stirling Radioisotope Generator (SRG110) for possible use on future NASA Space Science missions is being developed by the Department of Energy, Lockheed Martin, Stirling Technology Company (STC), and NASA Glenn Research Center (GRC). Potential mission use includes providing spacecraft onboard electric power for deep space missions and power for unmanned Mars rovers. GRC is conducting an in-house supporting technology project to assist in SRG110 development. One-, three-, and six-month heater head structural benchmark tests have been completed in support of a heater head life assessment. Testing is underway to evaluate the key epoxy bond of the permanent magnets to the linear alternator stator lamination stack. GRC has completed over 10,000 hours of extended duration testing of the Stirling convertors for the SRG110, and a three-year test of two Stirling convertors in a thermal vacuum environment will be starting shortly. GRC is also developing advanced technology for Stirling convertors, aimed at substantially improving the specific power and efficiency of the convertor and the overall generator. Sunpower, Inc. has begun the development of a lightweight Stirling convertor, under a NASA Research Announcement (NRA) award, that has the potential to double the system specific power to about 8 We/kg. GRC has performed random vibration testing of a lower-power version of this convertor to evaluate robustness for surviving launch vibrations. STC has also completed the initial design of a lightweight convertor. Status of the development of a multi-dimensional computational fluid dynamics code and high-temperature materials work on advanced superalloys, refractory metal alloys, and ceramics are also discussed.

Thieme, Lanny G.↗
NASA NTRS2005

Supporting Development for the Stirling Radioisotope Generator and Advanced Stirling Technology Development at NASA Glenn

A high-efficiency, 110-W(sub e) (watts electric) Stirling Radioisotope Generator (SRG110) for possible use on future NASA Space Science missions is being developed by the Department of Energy, Lockheed Martin, Stirling Technology Company (STC), and NASA Glenn Research Center (GRC). Potential mission use includes providing spacecraft onboard electric power for deep space missions and power for unmanned Mars rovers. GRC is conducting an in-house supporting technology project to assist in SRG110 development. One-, three-, and six-month heater head structural benchmark tests have been completed in support of a heater head life assessment. Testing is underway to evaluate the key epoxy bond of the permanent magnets to the linear alternator stator lamination stack. GRC has completed over 10,000 hours of extended duration testing of the Stirling convertors for the SRG110, and a three-year test of two Stirling convertors in a thermal vacuum environment will be starting shortly. GRC is also developing advanced technology for Stirling convertors, aimed at substantially improving the specific power and efficiency of the convertor and the overall generator. Sunpower, Inc. has begun the development of a lightweight Stirling convertor, under a NASA Research Announcement (NRA) award, that has the potential to double the system specific power to about 8 W(sub e) per kilogram. GRC has performed random vibration testing of a lowerpower version of this convertor to evaluate robustness for surviving launch vibrations. STC has also completed the initial design of a lightweight convertor. Status of the development of a multi-dimensional computational fluid dynamics code and high-temperature materials work on advanced superalloys, refractory metal alloys, and ceramics are also discussed.

Thieme, Lanny G.↗
NASA NTRS1990

LARC-IA: A flexible backbone polyimide

A new linear, aromatic, thermoplastic polyimide, prepared from oxydiphthalic anhydride (ODPA) and 3,4'-oxydianiline (ODA) in diglyme and identified as LARC-IA, was synthesized and evaluated. The monomers are relatively inexpensive and physiologically safe. Molecular weight was controlled by use of a monofunctional anhydride, phthalic anhydride (PA), in order to promote controlled flow and wetting properties. The polymer is considered a safe alternative to commercially available LARC-TPI which is prepared with an expensive diamine of uncertain carcinogenicity. The evaluation was based primarily on the polymer's adhesive properties as determined by thermal and water boil exposure of lap shear specimens. Strengths were determined at room temperature, 177, 204 and 232 C before and after exposure to determine the adhesive system's durability to adverse environments over a period of time. Other properties (FWT, G(1c), film and composite properties) were examined which were determined to be typical of a high temperature polyimide. Results of the study show a favorable comparison to LARC-TPI, a commercially available polyimide.

Progar, Donald J.↗
NASA NTRS2008

Self-Deploying Trusses Containing Shape-Memory Polymers

Composite truss structures are being developed that can be compacted for stowage and later deploy themselves to full size and shape. In the target applications, these smart structures will precisely self-deploy and support a large, lightweight space-based antenna. Self-deploying trusses offer a simple, light, and affordable alternative to articulated mechanisms or inflatable structures. The trusses may also be useful in such terrestrial applications as variable-geometry aircraft components or shelters that can be compacted, transported, and deployed quickly in hostile environments. The truss technology uses high-performance shape-memory-polymer (SMP) thermoset resin reinforced with fibers to form a helical composite structure. At normal operating temperatures, the truss material has the structural properties of a conventional composite. This enables truss designs with required torsion, bending, and compression stiffness. However, when heated to its designed glass transition temperature (Tg), the SMP matrix acquires the flexibility of an elastomer. In this state, the truss can be compressed telescopically to a configuration encompassing a fraction of its original volume. When cooled below Tg, the SMP reverts to a rigid state and holds the truss in the stowed configuration without external constraint. Heating the materials above Tg activates truss deployment as the composite material releases strain energy, driving the truss to its original memorized configuration without the need for further actuation. Laboratory prototype trusses have demonstrated repeatable self-deployment cycles following linear compaction exceeding an 11:1 ratio (see figure).

Schueler, Robert M.↗
NASA NTRS2011

Modeling Geometric Arrangements of TiO2-Based Catalyst Substrates and Isotropic Light Sources to Enhance the Efficiency of a Photocatalystic Oxidation (PCO) Reactor

The closed confined environments of the ISS, as well as in future spacecraft for exploration beyond LEO, provide many challenges to crew health. One such challenge is the availability of a robust, energy efficient, and re-generable air revitalization system that controls trace volatile organic contaminants (VOCs) to levels below a specified spacecraft maximum allowable concentration (SMAC). Photocatalytic oxidation (PCO), which is capable of mineralizing VOCs at room temperature and of accommodating a high volumetric flow, is being evaluated as an alternative trace contaminant control technology. In an architecture of a combined air and water management system, placing a PCO unit before a condensing heat exchanger for humidity control will greatly reduce the organic load into the humidity condensate loop ofthe water processing assembly (WPA) thereby enhancing the life cycle economics ofthe WPA. This targeted application dictates a single pass efficiency of greater than 90% for polar VOCs. ~ Although this target was met in laboratory bench-scaled reactors, no commercial or SBIR-developed prototype PCO units examined to date have achieved this goal. Furthermore, the formation of partial oxidation products (e.g., acetaldehyde) was not eliminated. It is known that single pass efficiency and partial oxidation are strongly dependent upon the contact time and catalyst illumination, hence the requirement for an efficient reactor design. The objective of this study is to maximize the apparent contact time and illuminated catalyst surface area at a given reactor volume and volumetric flow. In this study, a Ti02-based photocatalyst is assumed to be immobilized on porous substrate panels and illumination derived from linear isotropic light sources. Mathematical modeling using computational fluid dynamics (CFD) analyses were performed to investigate the effect of: 1) the geometry and configuration of catalyst-coated substrate panels, 2) porosity of the supporting substrate, and 3) varying the light source and spacing on contact time and illuminated catalyst area.

Richards, Jeffrey T.↗
NASA NTRS1990

A heat receiver design for solar dynamic space power systems

An advanced heat pipe receiver designed for a solar dynamic space power system is described. The power system consists of a solar concentrator, solar heat receiver, Stirling heat engine, linear alternator and waste heat radiator. The solar concentrator focuses the sun's energy into a heat receiver. The engine and alternator convert a portion of this energy to electric power and the remaining heat is rejected by a waste heat radiator. Primary liquid metal heat pipes transport heat energy to the Stirling engine. Thermal energy storage allows this power system to operate during the shade portion of an orbit. Lithium fluoride/calcium fluoride eutectic is the thermal energy storage material. Thermal energy storage canisters are attached to the midsection of each heat pipe. The primary heat pipes pass through a secondary vapor cavity heat pipe near the engine and receiver interface. The secondary vapor cavity heat pipe serves three important functions. First, it smooths out hot spots in the solar cavity and provides even distribution of heat to the engine. Second, the event of a heat pipe failure, the secondary heat pipe cavity can efficiently transfer heat from other operating primary heat pipes to the engine heat exchanger of the defunct heat pipe. Third, the secondary heat pipe vapor cavity reduces temperature drops caused by heat flow into the engine. This unique design provides a high level of reliability and performance.

Baker, Karl W.↗
NASA NTRSDate not supplied

Evaluation of Automotive Grade Resistors for Space Flight

Over the past decade, electronic, electrical, and electromechanical (EEE) parts for space applications have undergone significant changes, largely driven by CubeSat and commercial space developers pushing the boundaries on the utilization of commercial parts in space. Global product shortages and shipping delays are still impacting space flight project deadlines. Many projects have turned to automotive grade resistors as an alternate to their MILSPEC counterparts to fulfill requirements. In addition, automotive grade resistors may offer designers a wider range of parts to consider. A recent NASA study recommended the use of high-volume manufactured commercial components for space applications provided these components show evidence of stringent fabrication controls and thorough reliability monitoring practices. Automotive grade components have stringent qualification requirements per the Automotive Electronic Council (AEC). However, the end user usually does not have insight into the practices the manufacturer may use to reduce/eliminate infant mortality nor for compliance to all datasheet specifications. Screening, Life and Accelerated Life testing on a set of standard automotive-grade chip resistors is proposed to evaluate the reliability of these components. Requirements from both the AEC-Q (Automotive Electronic Council Qualification) and EEE-INST-002 (Instructions for EEE Parts Selection, Screening, Qualification, and Derating) for resistors is compared and discussed. The resistors have been tested by using a modified methodology from EEEINST-002 to evaluate their reliability for space flight projects. The findings of this study indicate that the underlying degradation mechanisms at rated temperature and power are best represented by power law models with a fitted exponent between 0 and 1. A linear model is more conservative which compensates for potential model uncertainty given the wide range of design and materials used in automotive resistors, while still providing useful long-term resistance drift estimates. No electrical anomalies or failures were observed throughout the 1000-hour Life Tests other than small in tolerance resistance drift aging. Degradation models were utilized to quantify and extrapolate the long-term resistance drift under operating conditions for the components. The models demonstrated that some automotive-grade resistors are likely to operate 10 years at nominal usage conditions while others might fail earlier.

Zainab Abdullahi↗
NASA NTRSDate not supplied

Evaluation of Automotive Grade Resistors for Space Flight

Over the past decade, electronic, electrical, and electromechanical (EEE) parts for space applications have undergone significant changes, largely driven by CubeSat and commercial space developers pushing the boundaries on the utilization of commercial parts in space. Global product shortages and shipping delays are still impacting space flight project deadlines. Many projects have turned to automotive grade resistors as an alternate to their MIL-SPEC counterparts to fulfill requirements. In addition, automotive grade resistors may offer designers a wider range of parts to consider. A recent NASA study recommended the use of high-volume manufactured commercial components for space applications provided these components show evidence of stringent fabrication controls and thorough reliability monitoring practices [1]. Automotive grade components have stringent qualification requirements per the Automotive Electronic Council (AEC). However, the end user usually does not have insight into the practices the manufacturer may use to reduce/eliminate infant mortality nor for compliance to all datasheet specifications. Screening, Life and Accelerated Life testing on a set of standard automotive-grade chip resistors is proposed to evaluate the reliability of these components. Requirements from both the AEC-Q (Automotive Electronic Council Qualification) and EEE-INST-002 (Instructions for EEE Parts Selection, Screening, Qualification, and Derating) for resistors is compared and discussed. The resistors have been tested by using a modified methodology from EEE-INST-002 to evaluate their reliability for space flight projects. The findings of this study indicate that the underlying degradation mechanisms at rated temperature and power are best represented by power law models with a fitted exponent between 0 and 1. A linear model is more conservative which compensates for potential model uncertainty given the wide range of design and materials used in automotive resistors, while still providing useful long-term resistance drift estimates. No electrical anomalies or failures were observed throughout the 1,000-hour Life Tests other than small in tolerance resistance drift aging. Degradation models were utilized to quantify and extrapolate the long-term resistance drift under operating conditions for the components. The models demonstrated that some automotive-grade resistors are likely to operate 10 years at nominal usage conditions while others might fail earlier.

Zainab Abdullahi↗
NASA NTRS2012

Analyses of Cometary Silicate Crystals: DDA Spectral Modeling of Forsterite

Comets are the Solar System's deep freezers of gases, ices, and particulates that were present in the outer protoplanetary disk. Where comet nuclei accreted was so cold that CO ice (approximately 50K) and other supervolatile ices like ethane (C2H2) were preserved. However, comets also accreted high temperature minerals: silicate crystals that either condensed (greater than or equal to 1400 K) or that were annealed from amorphous (glassy) silicates (greater than 850-1000 K). By their rarity in the interstellar medium, cometary crystalline silicates are thought to be grains that formed in the inner disk and were then radially transported out to the cold and ice-rich regimes near Neptune. The questions that comets can potentially address are: How fast, how far, and over what duration were crystals that formed in the inner disk transported out to the comet-forming region(s)? In comets, the mass fractions of silicates that are crystalline, f_cryst, translate to benchmarks for protoplanetary disk radial transport models. The infamous comet Hale-Bopp has crystalline fractions of over 55%. The values for cometary crystalline mass fractions, however, are derived assuming that the mineralogy assessed for the submicron to micron-sized portion of the size distribution represents the compositional makeup of all larger grains in the coma. Models for fitting cometary SEDs make this assumption because models can only fit the observed features with submicron to micron-sized discrete crystals. On the other hand, larger (0.1-100 micrometer radii) porous grains composed of amorphous silicates and amorphous carbon can be easily computed with mixed medium theory wherein vacuum mixed into a spherical particle mimics a porous aggregate. If crystalline silicates are mixed in, the models completely fail to match the observations. Moreover, models for a size distribution of discrete crystalline forsterite grains commonly employs the CDE computational method for ellipsoidal platelets (c:a:b=8.14x8.14xl in shape with geometrical factors of x:y:z=1:1:10, Fabian et al. 2001; Harker et al. 2007). Alternatively, models for forsterite employ statistical methods like the Distribution of Hollow Spheres (Min et al. 2008; Oliveira et al. 2011) or Gaussian Random Spheres (GRS) or RGF (Gielen et al. 200S). Pancakes, hollow spheres, or GRS shapes similar to wheat sheaf crystal habit (e.g., Volten et al. 2001; Veihelmann et al. 2006), however, do not have the sharp edges, flat faces, and vertices seen in images of cometary crystals in interplanetary dust particles (IDPs) or in Stardust samples. Cometary forsterite crystals often have equant or tabular crystal habit (J. Bradley). To simulate cometary crystals, we have computed absorption efficiencies of forsterite using the Discrete Dipole Approximation (DDA) DDSCAT code on NAS supercomputers. We compute thermal models that employ a size distribution of discrete irregularly shaped forsterite crystals (nonspherical shapes with faces and vertices) to explore how crystal shape affects the shape and wavelength positions of the forsterite spectral features and to explore whether cometary crystal shapes support either condensation or annealing scenarios (Lindsay et al. 2012a, b). We find forsterite crystal shapes that best-fit comet Hale-Bopp are tetrahedron, bricks or brick platelets, essentially equant or tabular (Lindsay et al. 2012a,b), commensurate with high temperature condensation experiments (Kobatake et al. 2008). We also have computed porous aggregates with crystal monomers and find that the crystal resonances are amplified. i.e., the crystalline fraction is lower in the aggregate than is derived by fitting a linear mix of spectral features from discrete subcomponents, and the crystal resonances 'appear' to be from larger crystals (Wooden et al. 2012). These results may indicate that the crystalline mass fraction in comets with comae dominated by aggregates may be lower than deduced by popular methods that only emoy ensembles of discrete crystals.

Wooden, Diane↗
NASA NTRS2003

Three-Dimensional Magnetic Analysis Technique Developed for Evaluating Stirling Convertor Linear Alternators

The Department of Energy, the Stirling Technology Company (STC), and the NASA Glenn Research Center are developing Stirling convertors for Stirling radioisotope generators to provide electrical power for future NASA deep space missions. STC is developing the 55-We technology demonstration convertor (TDC) under contract to the Department of Energy. The Department of Energy recently named Lockheed Martin as the system integration contractor for the Stirling radioisotope generator development project. Lockheed Martin will develop the Stirling radioisotope generator engineering unit and has contract options to develop the qualification unit and the first flight unit. Glenn s role includes an in-house project to provide convertor, component, and materials testing and evaluation in support of the overall power system development. As a part of this work, Glenn has established an in-house Stirling research laboratory for testing, analyzing, and evaluating Stirling machines. STC has built four 55-We convertors for NASA, and these are being tested at Glenn. A cross-sectional view of the 55-We TDC is shown in the figure. Of critical importance to the successful development of the Stirling convertor for space power applications is the development of a lightweight and highly efficient linear alternator. In support, Glenn has been developing finite element analysis and finite element method tools for performing various linear alternator thermal and electromagnetic analyses and evaluating design configurations. A three-dimensional magnetostatic finite element model of STC's 55-We TDC linear alternator was developed to evaluate the demagnetization fields affecting the alternator magnets. Since the actual linear alternator hardware is symmetric to the quarter section about the axis of motion, only a quarter section of the alternator was modeled. The components modeled included the mover laminations, the neodymium-iron-boron magnets, the stator laminations, and the copper coils. The three-dimensional magnetostatic model was then coupled with a circuit simulator model of the alternator load and convertor controller. The coupled model was then used to generate alternator terminal voltage and current predictions. The predicted voltage and current waveforms agreed well with the experimental data, which tended to validate the accuracy of the coupled model. The model was then used to generate predictions of the demagnetization fields acting on the alternator magnets for the alternator under load. The preliminary model predictions indicate that the highest potential for demagnetization is along the inside surface of the uncovered magnets. The demagnetization field for the uncovered magnets when the mover is positioned at the end of a stroke is higher than it is when the mover is at the position of maximum induced voltage or maximum alternator current. Assuming normal load conditions, the model predicted that the onset of demagnetization is most likely to occur for magnet temperatures above 101 C.

Geng, Steven M.↗
NASA NTRS2008

5-kWe Free-piston Stirling Engine Convertor

The high reliability, long life, and efficient operation of Free-Piston Stirling Engines (FPSEs) make them an attractive power system to meet future space power requirements with less mass, better efficiency, and less total heat exchanger area than other power convertor options. FPSEs are also flexible in configuration as they can be coupled with many potential heat sources and various heat input systems, heat rejection systems, and power management and distribution systems. Development of a 5-kWe Stirling Convertor Assembly (SCA) is underway to demonstrate the viability of an FPSE for space power. The design is a scaled-down version of the successful 12.5-kWe Component Test Power Converter (CTPC) developed under NAS3-25463. The ultimate efficiency target is 25% overall convertor efficiency (electrical power out over heat in). For the single cylinder prototype now in development, cost and time constraints required use of economical and readily available materials (steel versus beryllium) and components (a commercially available linear alternator) and thus lower efficiency. The working gas is helium at 150 bar mean pressure. The design consists of a displacer suspended on internally pumped gas bearings and a power piston/alternator supported on flexures. Non-contacting clearance seals are used between internal volumes. Heat to and from the prototype convertor is done via pumped liquid loops passing through shell and tube heat exchangers. The preliminary and detail designs of the convertor, controller, and support systems (heating loop, cooling loop, and helium supply system) are complete and all hardware is on order. Assembly and test of the prototype at Foster- Miller is planned for early 2008, when work will focus on characterizing convertor dynamics and steady-state operation to determine maximum power output and system efficiency. The device will then be delivered to Auburn University where assessments will include start-up and shutdown characterization and transient response to temperature and load variations. Future activities may include testing at NASA GRC.

Chapman, Peter A.↗
NASA NTRS1997

Extraterrestrial Helium (He@C60) Trapped in Fullerenes in the Sudbury Impact Structure

Fullerenes (C60 and C70) have recently been identified in a shock-produced breccia (Onaping Formation) associated with the 1.85-Ga Sudbury Impact Crater. The presence of parts-per-million levels of fullerenes in this impact structure raises interesting questions about the processes that led to the formation of fullerenes and the potential for delivery of intact organic material to the Earth by a large bolide (e.g., asteroid or comet). Two possible scenarios for the presence of fullerenes in the Sudbury impact deposits are that (1) fullerenes are synthesized within the impact plume from the C contained in the bolide; or (2) fullerenes are already present in the bolide and survived the impact event. The correlation of C and trapped noble gas atoms in meteorites is well established. Primitive meteorites contain several trapped noble gas components that have anomalous isotopic compositions, some of which may have a presolar origin. Several C-bearing phases, including SiC, graphite, and diamond, have been recognized as carriers of trapped noble gases. It has also been suggested that fullerenes (C60 and C70) might be a carrier of noble gas components in carbonaceous chondrites. Recently, fullerenes have been detected in separate samples in the Allende meteorite. Carbon-60 is large enough to enclose the noble gases He, Ne, Ar, Kr, and Xe, but it is too small to contain diatomic gases such as N2 or triatomic gases such as CO2. Recent experimental work has demonstrated that noble gases of a specific isotopic composition can be introduced into synthetic fullerenes at high temperatures and pressures; these encapsulated gases can then be released by the breaking of one or more C bonds during step-heating under vacuum. These thermal-release patterns for He encapsulated within the C60 molecule (He@C60) are similar to the patterns for acid residues of carbonaceous chondrites, suggesting that fullerenes could be an additional carrier of trapped noble gases in acid residues of meteorites. Analysis and Results: In order to characterize the noble gas compositions of the Sudbury fullerenes, we undertook a systematic study of acid-resistant residues throughout the C-rich layer (Black member) of the Onaping Formation. Samples were demineralized and extracted using standard techniques. The Onaping extracts were analyzed using several techniques, including UV-Vis adsorption, electro spray mass spectrometry, and laser desorption (linear and reflectron) time-of-flight (TOF) mass spectrometry (LDMS). The Sudbury fullerenes were then separated and purified using HPLC coupled with a photo diode array detector. The HPLC extracts containing the purified fullerenes were loaded into a metal tube furnace within a glove box under a N atmosphere in preparation for noble gas analyses. The 3-He and 4-He content of the fullerene extracts was measured using previously reported standard techniques . Discussion: Fullerenes (C60 and C70) in the Sudbury Impact Structure have been found to contain trapped He with a 3-He/4-He ratio greater than 5 x 10(exp -4). The 3-He/4-He ratio exceeds the accepted solar value by more than 30% and is more than 10x higher than the maximum reported mantle value. Terrestrial nuclear reactions or cosmic-my bombardment are not sufficient to generate such a high ratio. The 3-He/4-He ratios in the Sudbury fullerenes are similar to those determined for interplanetary dust particles. The greater-than-solar ratios of 3-He/4-He in the Sudbury fullerenes may indicate a presolar origin, although alternative mechanisms occurring in the ISM to explain these high ratios (e.g., spallation reactions, selective He implantation, etc.) cannot be entirely ruled out. We are currently attempting to isolate enough fullerene material to measure anomalous Ne (or Kr or Xe) contained within the C60 (e.g., the "pure" 22-Ne component) and thus determine whether the Sudbury fullerenes are indeed presolar in origin.

Becker, L.↗
NASA NTRS2008

Compact, Highly Stable Ion Atomic Clock

A mercury-ion clock now at the breadboard stage of development (see figure) has a stability comparable to that of a hydrogen-maser clock: In tests, the clock exhibited an Allan deviation of between 2 x 10(exp -13) and 3 x 10(exp -13) at a measurement time of 1 second, averaging to about 10(exp -15) at 1 day. However, the clock occupies a volume of only about 2 liters . about a hundredth of the volume of a hydrogen-maser clock. The ion-handling parts of the apparatus are housed in a sealed vacuum tube, wherein only a getter pump is used to maintain the vacuum. Hence, this apparatus is a prototype of a generation of small, potentially portable high-precision clocks for diverse ground- and space-based navigation and radio science applications. Furthermore, this new ion-clock technology is about 100 times more stable and precise than the rubidium atomic clocks currently in use in the NAV STAR GPS Earth-orbiting satellites. In this clock, mercury ions are shuttled between a quadrupole and a 16-pole linear radio-frequency trap. In the quadrupole trap, the ions are tightly confined and optical state selection from a Hg-202 radio-frequency-discharge ultraviolet lamp is carried out. In the 16-pole trap, the ions are more loosely confined and atomic transitions resonant at frequency of about 40.507 GHz are interrogated by use of a microwave beam at that frequency. The trapping of ions effectively eliminates the frequency pulling caused by wall collisions inherent to gas-cell clocks. The shuttling of the ions between the two traps enables separation of the state-selection process from the clock microwave- resonance process, so that each of these processes can be optimized independently of the other. The basic ion-shuttling, two-trap scheme as described thus far is not new: it has been the basis of designs of prior larger clocks. The novelty of the present development lies in major redesigns of its physics package (the ion traps and the vacuum and optical subsystems) to effect the desired reduction of size to a volume of no more than a couple of liters. The redesign effort has included selection of materials for the vacuum tube, ion trap, and ultraviolet windows that withstand bakeout at a temperature of approx.450 C in preparation for sealing the tube to contain the vacuum. This part of the redesign effort follows the approach taken in the development of such other vacuum-tube electronic components as flight traveling- wave-tube amplifiers having operational and shelf lives as long as 15 years. The redesign effort has also included a thorough study of residual-gas-induced shifts of the ion-clock frequency and a study of alternative gases as candidates for use as a buffer gas within the sealed tube. It has been found that neon is more suitable than is helium, which has been traditionally used for this purpose, in that the pressure-induced frequency pulling by neon is between a third and a half of that of helium. In addition, because neon diffuses through solids much more slowly than does helium, the loss of neon by diffusion over the operational lifetime is expected to be negligible.

Prestage, John↗
NASA NTRS2005

Sol-Gel Process for Making Pt-Ru Fuel-Cell Catalysts

A sol-gel process has been developed as a superior alternative to a prior process for making platinum-ruthenium alloy catalysts for electro-oxidation of methanol in fuel cells. The starting materials in the prior process are chloride salts of platinum and ruthenium. The process involves multiple steps, is time-consuming, and yields a Pt-Ru product that has relatively low specific surface area and contains some chloride residue. Low specific surface area translates to incomplete utilization of the catalytic activity that might otherwise be available, while chloride residue further reduces catalytic activity ("poisons" the catalyst). In contrast, the sol-gel process involves fewer steps and less time, does not leave chloride residue, and yields a product of greater specific area and, hence, greater catalytic activity. In this sol-gel process (see figure), the starting materials are platinum(II) acetylacetonate [Pt(C5H7O2)2, also denoted Pt-acac] and ruthenium(III) acetylacetonate [Ru(C5H7O2)3, also denoted Ru-acac]. First, Pt-acac and Ru-acac are dissolved in acetone at the desired concentrations (typically, 0.00338 moles of each salt per 100 mL of acetone) at a temperature of 50 C. A solution of 25 percent tetramethylammonium hydroxide [(CH3)4NOH, also denoted TMAH] in methanol is added to the Pt-acac/Ruacac/ acetone solution to act as a high-molecular-weight hydrolyzing agent. The addition of the TMAH counteracts the undesired tendency of Pt-acac and Ru-acac to precipitate as separate phases during the subsequent evaporation of the solvent, thereby helping to yield a desired homogeneous amorphous gel. The solution is stirred for 10 minutes, then the solvent is evaporated until the solution becomes viscous, eventually transforming into a gel. The viscous gel is dried in air at a temperature of 170 C for about 10 hours. The dried gel is crushed to make a powder that is the immediate precursor of the final catalytic product. The precursor powder is converted to the final product in a controlled-atmosphere heat treatment. Desirably, the final product is a phase-pure (Pt phase only) Pt-Ru powder with a high specific surface area. The conditions of the controlled- atmosphere heat are critical for obtaining the aforementioned desired properties. A typical heat treatment that yields best results for a catalytic alloy of equimolar amounts of Pt and Ru consists of at least two cycles of heating to a temperature of 300 C and holding at 300 C for several hours, all carried out in an atmosphere of 1 percent O2 and 99 percent N2. The resulting powder consists of crystallites with typical linear dimensions of <10 nm. Tests have shown that the powder is highly effective in catalyzing the electro-oxidation of methanol.

Narayanan, Sekharipuram↗