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NASA NTRS2008

LiGa(OTf)(sub 4) as an Electrolyte Salt for Li-Ion Cells

Lithium tetrakis(trifluoromethane sulfo - nato)gallate [abbreviated "LiGa(OTf)4" (wherein "OTf" signifies trifluoro - methanesulfonate)] has been found to be promising as an electrolyte salt for incorporation into both liquid and polymer electrolytes in both rechargeable and non-rechargeable lithium-ion electrochemical cells. This and other ingredients have been investigated in continuing research oriented toward im proving the performances of rechargeable lithium-ion electrochemical cells, especially at low temperatures. This research at earlier stages, and the underlying physical and chemical principles, were reported in numerous previous NASA Tech Briefs articles. As described in more detail in those articles, lithiumion cells most commonly contain nonaqueous electrolyte solutions consisting of lithium hexafluorophosphate (LiPF6) dissolved in mixtures of cyclic and linear alkyl carbonates, including ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), and ethyl methyl carbonate (EMC). Although such LiPF6-based electrolyte solutions are generally highly ionically conductive and electrochemically stable, as needed for good cell performance, there is interest in identifying alternate lithium electrolyte salts that, relative to LiPF6, are more resilient at high temperature and are less expensive. Experiments have been performed on LiGa(OTf)4 as well as on several other candidate lithium salts in pursuit of this interest. As part of these experiments, LiGa(OTf)4 was synthesized by the reaction of Ga(OTf)3 with an equimolar portion of LiOTf in a solvent consisting of anhydrous acetonitrile. Evaporation of the solvent yielded LiGa(OTf)4 as a colorless crystalline solid. The LiGa(OTf)4 and the other salts were incorporated into solutions with PC and DMC. The resulting electrolyte solutions exhibited reasonably high ionic conductivities over a relatively wide temperature range down to 40 C (see figure). In cyclic voltammetry measurements, LiGa(OTf)4 and the other salts exhibited acceptably high electrochemical stability over the relatively wide potential window of 0 to 5 V versus Li+/Li. 13C nuclear-magneticresonance measurements yielded results that suggested that in comparison with the other candidate salts, LiGa(OTf)4 exhibits less ion pairing. Planned further development will include optimization of the salt and solvent contents of such electrolyte solutions and incorporation of LiGa(OTf)4 into gel and solid-state polymer electrolytes. Of the salts, LiGa(OTf)4 is expected to be especially desirable for incorporation into lithium polymer electrolytes, wherein decreased ion pairing is advantageous and the large delocalized anions can exert a plasticizing effect.

Reddy, V. Prakash↗

NASA NTRS2007

Thermal Conductivity of Ethylene Vinyl Acetate Copolymer/Nanofiller Blends

To reduce weight and increase the mobility, comfort, and performance of future spacesuits, flexible, thermally conductive fabrics and plastic tubes are needed for the Liquid Cooling and Ventilation Garment. Such improvements would allow astronauts to operate more efficiently and safely for extended extravehicular activities. As an approach to raise the thermal conductivity (TC) of an ethylene vinyl acetate copolymer (Elvax 260), it was compounded with three types of carbon based nanofillers: multi-walled carbon nanotubes (MWCNTs), vapor grown carbon nanofibers (CNFs), and expanded graphite (EG). In addition, other nanofillers including metallized CNFs, nickel nanostrands, boron nitride, and powdered aluminum were also compounded with Elvax 260 in the melt at various loading levels. In an attempt to improve compatibility between Elvax 260 and the nanofillers, MWCNTs and EG were modified by surface coating and through noncovalent and covalent attachment of organic molecules containing alkyl groups. Ribbons of the nanocomposites were extruded to form samples in which the nanofillers were aligned in the direction of flow. Samples were also fabricated by compression molding to yield nanocomposites in which the nanofillers were randomly oriented. Mechanical properties of the aligned samples were determined by tensile testing while the degree of dispersion and alignment of nanoparticles were investigated using high-resolution scanning electron microscopy. TC measurements were performed using a laser flash (Nanoflash ) technique. TC of the samples was measured in the direction of, and perpendicular to, the alignment direction. Additionally, tubing was also extruded from select nanocomposite compositions and the TC and mechanical flexibility measured.

Ghose, S.↗

NASA NTRS2007

Thermal Conductivity of Ethylene Vinyl Acetate Copolymer/Carbon Nanofiller Blends

Ghose, S.↗

NASA NTRS2007

Thermal Conductivity of Ethylene Vinyl Acetate Copolymer/Nanofiller Blends

To reduce weight and increase the mobility, comfort, and performance of future spacesuits, flexible, thermally conductive fabrics and plastic tubes are needed for the Liquid Cooling and Ventilation Garment. Such improvements would allow astronauts to operate more efficiently and safely for extended extravehicular activities. As an approach to raise the thermal conductivity (TC) of an ethylene vinyl acetate copolymer (Elvax(TM)260), it was compounded with three types of carbon based nanofillers: multi-walled carbon nanotubes (MWCNTs), vapor grown carbon nanofibers (CNFs), and expanded graphite (EG). In addition, other nanofillers including metallized CNFs, nickel nanostrands, boron nitride, and powdered aluminum were also compounded with Elvax(TM) 260 in the melt at various loading levels. In an attempt to improve compatibility between Elvax 260 and the nanofillers, MWCNTs and EG were modified by surface coating and through noncovalent and covalent attachment of organic molecules containing alkyl groups. Ribbons of the nanocomposites were extruded to form samples in which the nanofillers were aligned in the direction of flow. Samples were also fabricated by compression molding to yield nanocomposites in which the nanofillers were randomly oriented. Mechanical properties of the aligned samples were determined by tensile testing while the degree of dispersion and alignment of nanoparticles were investigated using high-resolution scanning electron microscopy. TC measurements were performed using a laser flash (Nanoflash(TM)) technique. TC of the samples was measured in the direction of, and perpendicular to, the alignment direction. Additionally, tubing was also extruded from select nanocomposite compositions and the TC and mechanical flexibility measured.

Ghose, Sayata↗

NASA NTRS2015

Analyses of Hubble Space Telescope Aluminized-Teflon Multilayer Insulation Blankets Retrieved After 19 Years of Space Exposure

Since its launch in April 1990, the Hubble Space Telescope (HST) has made many important observations from its vantage point in low Earth orbit (LEO). However, as seen during five servicing missions, the outer layer of multilayer insulation (MLI) has become increasingly embrittled and has cracked in many areas. In May 2009, during the 5th servicing mission (called SM4), two MLI blankets were replaced with new insulation and the space-exposed MLI blankets were retrieved for degradation analyses by teams at NASA Glenn Research Center (GRC) and NASA Goddard Space Flight Center (GSFC). The retrieved MLI blankets were from Equipment Bay 8, which received direct sunlight, and Equipment Bay 5, which received grazing sunlight. Each blanket was divided into several regions based on environmental exposure and/or physical appearance. The aluminized-Teflon (DuPont, Wilmington, DE) fluorinated ethylene propylene (Al-FEP) outer layers of the retrieved MLI blankets have been analyzed for changes in optical, physical, and mechanical properties, along with chemical and morphological changes. Pristine and as-retrieved samples (materials) were heat treated to help understand degradation mechanisms. When compared to pristine material, the analyses have shown how the Al-FEP was severely affected by the space environment. Most notably, the Al-FEP was highly embrittled, fracturing like glass at strains of 1 to 8 percent. Across all measured properties, more significant degradation was observed for Bay 8 material as compared to Bay 5 material. This paper reviews the tensile and bend-test properties, density, thickness, solar absorptance, thermal emittance, x-ray photoelectron spectroscopy (XPS) and energy dispersive spectroscopy (EDS) elemental composition measurements, surface and crack morphologies, and atomic oxygen erosion yields of the Al-FEP outer layer of the retrieved HST blankets after 19 years of space exposure.

Radiation↗

NASA NTRS1993

Fuel-rich catalytic combustion of a high density fuel

Fuel-rich catalytic combustion (ER is greater than 4) of the high density fuel exo-tetrahydrocyclopentadiene (JP-10) was studied over the equivalence ratio range 5.0 to 7.6, which yielded combustion temperatures of 1220 to 1120 K. The process produced soot-free gaseous products similar to those obtained with iso-octane and jet-A in previous studies. The measured combustion temperature agreed well with that calculated assuming soot was not a combustion product. The process raised the effective hydrogen/carbon (H/C) ratio from 1.6 to over 2.0, thus significantly improving the combustion properties of the fuel. At an equivalence ratio near 5.0, about 80 percent of the initial fuel carbon was in light gaseous products and about 20 percent in larger condensable molecules. Fuel-rich catalytic combustion has now been studied for three fuels with H/C ratios of 2.25 (iso-octane), 1.92 (jet-A), and 1.6 (JP-10). A comparison of the product distribution of these fuels shows that, in general, the measured concentrations of the combustion products were monotonic functions of the H/C ratio with the exception of hydrogen and ethylene. In these cases, data for JP-10 fell between iso-octane and jet-A rather than beyond jet-A. It is suggested that the ring cross-linking structure of JP-10 may be responsible for this behavior. All the fuels studied showed that the largest amounts of small hydrocarbon molecules and the smallest amounts of large condensable molecules occurred at the lower equivalence ratios. This corresponds to the highest combustion temperatures used in these studies. Although higher temperatures may improve this mix, the temperature is limited. First, the life of the present catalyst would be greatly shortened when operated at temperatures of 1300 K or greater. Second, fuel-rich catalytic combustion does not produce soot because the combustion temperatures used in the experiments were well below the threshold temperature (1350 K) for the formation of soot. Increasing the temperature above this value would remove the soot-free nature of the process. Since all the fuels studied show a similar breakdown of the primary fuel into smaller molecular combustion products, this technique can be applied to all hydrocarbon fuels.

Brabbs, Theodore A.↗

NASA NTRS2016

Erosion Results of the MISSE 7 Polymers Experiment and Zenith Polymers Experiment After 1.5 Years of Space Exposure

Polymers and other oxidizable materials on the exterior of spacecraft in the low Earth orbit (LEO) space environment can be eroded due to reaction with atomic oxygen (AO). Therefore, in order to design durable spacecraft it is important to know the LEO AO erosion yield (E(sub y), volume loss per incident oxygen atom) of materials susceptible to AO reaction. Two spaceflight experiments, the Polymers Experiment and the Zenith Polymers Experiment, were developed to determine the AO E(sub y) of various polymers flown in ram, wake or zenith orientations in LEO. These experiments were flown as part of the Materials International Space Station Experiment 7 (MISSE 7) mission for 1.5 years on the exterior of the International Space Station (ISS). The experiments included Kapton H(TradeMark) witness samples for AO fluence determination in ram and zenith orientations. The Polymers Experiment also included samples to determine whether AO erosion of high and low ash containing polymers is dependent on fluence. This paper provides an overview of the MISSE 7 mission, a description of the flight experiments with details on the polymers flown, the characterization techniques used, the AO fluence for each exposure orientation, and the LEO E(sub y) results. The E(sub y) values ranged from 7.99x10(exp -28)cu cm/atom for TiO2/Al2O3 coated Teflon(TradeMark) fluorinated ethylene propylene (FEP) flown in the ram orientation to 1.22x10(exp -23cu cm/atom for polyvinyl alcohol (PVOH) flown in the zenith orientation. The E(sub y) of similar samples flown in different orientations has been compared to help determine solar exposure and associated heating effects on AO erosion. The E(sub y) data from these ISS spaceflight experiments provides valuable information for LEO spacecraft design purposes.

Teflon↗

NASA NTRS1998

A Comparison of Space and Ground Based Facility Environmental Effects for FEP Teflon

Fluorinated Ethylene Propylene (FEP) Teflon is widely used as a thermal control material for spacecraft, however, it is susceptible to erosion, cracking, and subsequent mechanical failure in low Earth orbit. One of the difficulties in determining whether FEP Teflon will survive during a mission is the wide disparity of erosion rates observed for this material in space and in ground based facilities. Each environment contains different levels of atomic oxygen, ions, and vacuum ultraviolet (VUV) radiation in addition to parameters such as the energy of the arriving species and temperature. These variations make it difficult to determine what is causing the observed differences in erosion rates. This paper attempts to narrow down which factors affect the erosion rate of FEP Teflon through attempting to change only one environmental constituent at a time. This was attempted through the use of a single simulation facility (plasma asher) environment with a variety of Faraday cages and VUV transparent windows. Isolating one factor inside of a radio frequency (RF) plasma proved to be very difficult. Two observations could be made. First, it appears that the erosion yield of FEP Teflon with respect to that of polyimide Kapton is not greatly affected by the presence or lack of VUV radiation present in the RF plasma and the relative erosion yield for the FEP Teflon may decrease with increasing fluence. Second, shielding from charged particles appears to lower the relative erosion yield of the FEP to approximately that observed in space, however it is difficult to determine for sure whether ions, electrons, or some other components are causing the enhanced erosion.

Rutledge, Sharon K.↗

NASA NTRS2010

Optimized Li-Ion Electrolytes Containing Fluorinated Ester Co-Solvents

A number of experimental lithium-ion cells, consisting of MCMB (meso-carbon microbeads) carbon anodes and LiNi(0.8)Co(0.2)O2 cathodes, have been fabricated with increased safety and expanded capability. These cells serve to verify and demonstrate the reversibility, low-temperature performance, and electrochemical aspects of each electrode as determined from a number of electrochemical characterization techniques. A number of Li-ion electrolytes possessing fluorinated ester co-solvents, namely trifluoroethyl butyrate (TFEB) and trifluoroethyl propionate (TFEP), were demonstrated to deliver good performance over a wide temperature range in experimental lithium-ion cells. The general approach taken in the development of these electrolyte formulations is to optimize the type and composition of the co-solvents in ternary and quaternary solutions, focusing upon adequate stability [i.e., EC (ethylene carbonate) content needed for anode passivation, and EMC (ethyl methyl carbonate) content needed for lowering the viscosity and widening the temperature range, while still providing good stability], enhancing the inherent safety characteristics (incorporation of fluorinated esters), and widening the temperature range of operation (the use of both fluorinated and non-fluorinated esters). Further - more, the use of electrolyte additives, such as VC (vinylene carbonate) [solid electrolyte interface (SEI) promoter] and DMAc (thermal stabilizing additive), provide enhanced high-temperature life characteristics. Multi-component electrolyte formulations enhance performance over a temperature range of -60 to +60 C. With the need for more safety with the use of these batteries, flammability was a consideration. One of the solvents investigated, TFEB, had the best performance with improved low-temperature capability and high-temperature resilience. This work optimized the use of TFEB as a co-solvent by developing the multi-component electrolytes, which also contain non-halogenated esters, film forming additives, thermal stabilizing additives, and flame retardant additives. Further optimization of these electrolyte formulations is anticipated to yield improved performance. It is also anticipated that much improved performance will be demonstrated once these electrolyte solutions are incorporated into hermetically sealed, large capacity prototype cells, especially if effort is devoted to ensure that all electrolyte components are highly pure.

Prakash, G. K. Surya↗

NASA NTRS2017

Erosion Results of the MISSE 8 Polymers Experiment After 2 Years of Space Exposure on the International Space Station

Polymers and other oxidizable materials on the exterior of spacecraft in the low Earth orbit (LEO) space environment can be eroded due to reaction with atomic oxygen (AO). Therefore, in order to design durable spacecraft, it is important to know the LEO AO erosion yield (E(sub y), volume loss per incident oxygen atom) of materials susceptible to AO reaction. A spaceflight experiment, called the Polymers Experiment, which contained 42 samples, was developed to determine the effect of solar exposure on the AO E(sub y) of fluoropolymers flown in ram, wake, or zenith orientations. The Polymers Experiment was exposed to the LEO space environment on the exterior of the International Space Station (ISS) as part of the Materials International Space Station Experiment 8 (MISSE 8) mission. The MISSE 8 mission included samples flown in a zenith/nadir orientation for 2.14 years in the MISSE 8 Passive Experiment Container (PEC), and samples flown in a ram/wake orientation for 2.0 years in the Optical Reflector Materials Experiment-III (ORMatEIII) tray. The experiment included Kapton H (Registered Trademark) witness samples for AO fluence determination in each orientation. This paper provides an overview of the MISSE 8 mission, a description of the flight experiment with details on the polymers flown, the characterization techniques used, the AO fluence for each exposure orientation, and the LEO E(sub y) results. The E(sub y) of Teflon fluorinated ethylene propylene (FEP) samples flown in ram, wake, and zenith orientations have been compared, and the E(sub y) was found to be highly dependent on orientation and therefore environmental exposure. The FEP E(sub y) was found to directly correlate with the solar exposure/AO fluence ratio showing the effect of solar radiation and/or heating due to solar exposure on FEP erosion. In addition, back-surface carbon painted FEP (C-FEP) flown in the zenith orientation had a significantly higher E(sub y) than clear FEP or Al-FEP further indicating that heating has a significant impact on the erosion of FEP. This experiment provides valuable LEO flight data on the erosion of Teflon FEP, a commonly used spacecraft thermal insulation.

Teflon↗