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NASA NTRS2005

New Aptes Cross-linked Polymers from Poly(ethylene oxide)s and Cyanuric Chloride for Lithium Batteries

A new series of polymer electrolytes for use as membranes for lithium batteries are described. Electrolytes were made by polymerization between cyanuric chloride and diamino-terminated poly(ethylene oxide)s, followed by cross-linking via a sol-gel process. Thermal analysis and lithium conductivity of freestanding polymer films were studied. The effects of several variables on conductivity were investigated, such as length of backbone PEO chain, length of branching PEO chain, extent of branching, extent of cross-linking, salt content, and salt counterion. Polymer films with the highest percentage of PEO were found to be the most conductive, with a maximum lithium conductivity of 3.9 x 10(exp -5) S/cm at 25 C. Addition of plasticizer to the dry polymers increased conductivity by an order of magnitude.

Tigelaar, Dean M.↗

NASA NTRS1994

Dielectric Properties of Poly(ethylene oxide) from Molecular Dynamics Simulations

The order, conformations and dynamics of poly(oxyethylene) (POE) melts have been investigated through molecular dynamics simulations. The potential energy functions were determined from detailed ab initio electronic structure calculations of the conformational energies of the model molecules 1,2-dimethoxyethane (DME) and diethylether. The x-ray structure factor for POE from simulation will be compared to experiment. In terms of conformation, simulations reveal that chains are extended in the melt relative to isolated chains due to the presence of strong intermolecular O...H interactions, which occur at the expense of intramolecular O...H interactions. Conformational dynamics about the C-C bond were found to be significantly faster than in polymethylene, while conformational dynamics about the C-O bond even faster than the C-C dynamics. The faster local dynamics in POE relative to polymethylene is consistent with C-13 NMR spin-lattice relaxation experiments. Conformational transitions showed significant second-neighbor correlation, as was found for polymethylene. This correlation of transitions with C-C neighbors was found to be reduced relative to C-O neighbors. Dielectric relaxation from simulation will also be compared with experiment.

Smith, Grant D.↗

NASA NTRS2003

Design of Hybrid Solid Polymer Electrolytes: Structure and Properties

This paper reports synthesis, structure, and properties of novel hybrid solid polymer electrolytes (SPE's) consisting of organically modified aluminosilica (OM-ALSi), formed within a poly(ethylene oxide)-in-salt (Li triflate) phase. To alter the structure and properties we fused functionalized silanes containing poly(ethylene oxide) (PEO) tails or CN groups.

Bronstein, Lyudmila M.↗

NASA NTRS2007

Composite Electrolytes for Lithium Batteries: Ionic Liquids in APTES Crosslinked Polymers

Solvent free polymer electrolytes were made consisting of Li(+) and pyrrolidinium salts of trifluoromethanesulfonimide added to a series of hyperbranched poly(ethylene oxide)s (PEO). The polymers were connected by triazine linkages and crosslinked by a sol-gel process to provide mechanical strength. The connecting PEO groups were varied to help understand the effects of polymer structure on electrolyte conductivity in the presence of ionic liquids. Polymers were also made that contain poly(dimethylsiloxane) groups, which provide increased flexibility without interacting with lithium ions. When large amounts of ionic liquid are added, there is little dependence of conductivity on the polymer structure. However, when smaller amounts of ionic liquid are added, the inherent conductivity of the polymer becomes a factor. These electrolytes are more conductive than those made with high molecular weight PEO imbibed with ionic liquids at ambient temperatures, due to the amorphous nature of the polymer.

Tigelaar, Dean M.↗

NASA NTRS2009

Effects of Temperature on Polymer/Carbon Chemical Sensors

Experiments were conducted on the effects of temperature, polymer molecular weight, and carbon loading on the electrical resistances of polymer/carbon-black composite films. The experiment were performed in a continuing effort to develop such films as part of the JPL Electronic Nose (ENose), that would be used to detect, identify, and quantify parts-per-million (ppm) concentration levels of airborne chemicals in the space shuttle/space station environments. The polymers used in this study were three formulations of poly(ethylene oxide) [PEO] that had molecular weights of 20 kilodaltons, 600 kilodaltons, and 1 megadalton, respectively. The results of one set of experiments showed a correlation between the polymer molecular weight and the percolation threshold. In a second set of experiments, differences among the temperature dependences of resistance were observed for different carbon loadings; these differences could be explained by a change in the conduction mechanism. In a third set of experiments, the responses of six different polymer/carbon composite sensors to three analytes (water vapor, methanol, methane) were measured as a function of temperature (28 to 36 C). For a given concentration of each analyte, the response of each sensor decreased with increasing temperature, in a manner different from those of the other sensors.

Manfireda, Allison↗

NASA NTRS2007

Norbornene-Based Polymer Electrolytes for Lithium Cells

Norbornene-based polymers have shown promise as solid electrolytes for lithium-based rechargeable electrochemical cells. These polymers are characterized as single-ion conductors. Single-ion-conducting polymers that can be used in lithium cells have long been sought. Single-ion conductors are preferred to multiple-ion conductors as solid electrolytes because concentration gradients associated with multiple-ion conduction lead to concentration polarization. By minimizing concentration polarization, one can enhance charge and discharge rates. Norbornene sulfonic acid esters have been synthesized by a ring-opening metathesis polymerization technique, using ruthenium-based catalysts. The resulting polymer structures (see figure) include sulfonate ionomers attached to the backbones of the polymer molecules. These molecules are single-ion conductors in that they conduct mobile Li+ ions only; the SO3 anions in these polymers, being tethered to the backbones, do not contribute to ionic conduction. This molecular system is especially attractive in that it is highly amenable to modification through functionalization of the backbone or copolymerization with various monomers. Polymers of this type have been blended with poly(ethylene oxide) to lend mechanical integrity to free-standing films, and the films have been fabricated into solid polymer electrolytes. These electrolytes have been demonstrated to exhibit conductivity of 2 10(exp -5)S/cm (which is high, relative to the conductivities of other solid electrolytes) at ambient temperature, plus acceptably high stability. This type of norbornene-based polymeric solid electrolyte is in the early stages of development. Inasmuch as the method of synthesis of these polymers is inherently flexible and techniques for the fabrication of the polymers into solid electrolytes are amenable to optimization, there is reason to anticipate further improvements.

Cheung, Iris↗

NASA NTRS2003

Electrical Characterization and Morphological Studies of Conducting Polymer Nanofibers

Doped polyaniline blended with poly(ethylene oxide) has been electrospun in air to give fibers with diameters in the range 3 nm 200 nm. These fibers were captured on wafers of degenerately doped Si/SiO2 by placing the wafer in the path of the fiber jet formed during the electrospinning process. Individual fibers were contacted using shadow mask evaporation and were also captured on prepatterned wafers. Fibers having diameters greater than 100 nm show a slight increase in the conductivity as compared to the bulk film, while fibers with diameters less than 30 nm had lower conductivity than the bulk. Data on Scanning Conductance Microscopy along the length of individual fibers will be presented. For fibers where the diameter was not uniform, we found that below a certain diameter ( approx.15 nm) the fiber was less conducting as compared to thicker diameter fibers. Dependence of the fiber conductivity on a gate bias is underway and these results will also be presented.

Pinto, N. J.↗

NASA NTRS2011

Detection of Carbon Monoxide Using Polymer-Carbon Composite Films

A carbon monoxide (CO) sensor was developed that can be incorporated into an existing sensing array architecture. The CO sensor is a low-power chemiresistor that operates at room temperature, and the sensor fabrication techniques are compatible with ceramic substrates. Sensors made from four different polymers were tested: poly (4-vinylpryridine), ethylene-propylene-diene-terpolymer, polyepichlorohydrin, and polyethylene oxide (PEO). The carbon black used for the composite films was Black Pearls 2000, a furnace black made by the Cabot Corporation. Polymers and carbon black were used as received. In fact, only two of these sensors showed a good response to CO. The poly (4-vinylpryridine) sensor is noisy, but it does respond to the CO above 200 ppm. The polyepichlorohydrin sensor is less noisy and shows good response down to 100 ppm.

Homer, Margie L.↗

NASA NTRS1989

ESCA Study of Poly (Vinylidene Fluoride) Tetrafluoroethylene - Ethylene Copolymer and Polyethylene Exposed to Atomic Oxygen

The ESCA (electron spectroscopy for chemical analysis) spectra of films of poly(vinylidene fluoride) (PVDF), tetrafluoroethylene-ethylene copolymer (TFE/ET) and polyethylene (PE) exposed to atomic oxygen (O(P-3)), in or out of the glow of a radio-frequency O2 plasma, were compared. ESCA spectra of PE films exposed to (O(P-3)) in low Earth orbit (LEO) on the STS-8 Space Shuttle were also examined. Apart from O(P-3)-induced surface recession (etching), the various polymer films exhibited surface oxidation, which proceeded towards equilibrium saturation oxygen levels. The maximum surface oxygen uptakes for in-glow or out-of-glow exposures were in the order: PE greater than TFE/ET greater than PVDF; for PE itself, the oxygen uptakes were in the order: in glow greater than out of glow greater than LEO. Given prior ESCA data on poly(vinyl fluoride) and polytetrafluoroethylene films exposed to O(P-3), the extent of surface oxidation is seen to decrease regularly with increase in fluorine substitution in a family of ethylene-type polymers. (Keywords: ESCA; poly(vinylidene fluoride); tetrafluoroethylene ethylene copolymer; polyethylene; atomic oxygen; radio-frequency oxygen plasma; low Earth orbit)

Golub, Morton A.↗

NASA NTRS1996

Functional and Multifunctional Polymers: Materials for Smart Structures

The ultimate goal of the research in smart structures and smart materials is the development of a new generation of products/devices which will perform better than products/devices built from passive materials. There are a few examples of multilayer polymer systems which function as smart structures, e.g. a synthetic muscle which is a multilayer assembly of a poly(ethylene) layer, a gold layer, and a poly(pyrrole) layer immersed in a liquid electrolyte. Oxidation and reductions of the active pyrrole layer causes the assembly to reversibly deflect and mimic biological muscles. The drawback of such a setup is slow response times and the use of a liquid electrolyte. We have developed multifunctional polymers which will eliminate the use of a liquid electrolyte, and also because the functionalities of the polymers are within a few hundred angstroms, an improved response time to changes in the external field should be possible. Such multifunctional polymers may be classified as the futuristic 'smart materials.' These materials are composed of a number of different functionalities which work in a synergistic fashion to function as a device. The device performs on the application of an external field and such multifunctional polymers may be scientifically labeled as 'field responsive polymers.' Our group has undertaken a systematic approach to develop functional and multifunctional polymers capable of functioning as field responsive polymers. Our approach utilizes multicomponent polymer systems (block copolymers and graft copolymers), the strategy involves the preparation of block or graft copolymers where the functionalities are limited to different phases in a microphase separated system. Depending on the weight (or volume) fractions of each of the components, different microstructures are possible. And, because of the intimate contact between the functional components, an increase in the synergism between the functionalities may be observed. In this presentation, three examples of multifunctional polymers developed in our labs will be reported. The first class of multifunctional polymers are the microphase separated mixed (ionic and electronic) conducting or MIEC block copolymers. The second class being developed in our labs are the biocompatible conductive materials and the conductive fluids. The final class may be considered microwave active smart polymers.

Arnold, S.↗

NASA NTRS2019

Reinforcing Additives for Ice Adhesion Reduction Coatings

Adhesion of contaminants has been identified as a ubiquitous issue for aeronautic exterior surfaces. In-flight icing is particularly hazardous for all aircraft and can be experienced throughout the year under the appropriate environmental conditions. On larger vehicles, the accretion of ice could result in loss of lift, engine failure, and potentially loss of vehicle and life were it not for active deicing or anti-icing equipment. Smaller vehicles though cannot support the mass and mechanical complexity of active ice mitigating systems and thus must rely upon passive approaches or avoid icing conditions altogether. One approach that may be applicable to all aircraft is the use of coatings. Durability remains an issue and has prevented realization of coatings for leading edge contamination mitigation. In this work, epoxy coatings were generated as a passive approach for ice adhesion mitigation and methods to improve durability were evaluated. Highly cross-linked epoxy systems can be extremely rigid, which could have deleterious consequences regarding application as a leading edge coating. Incorporation of flexible species, such as poly(ethylene glycol) may improve coating toughness.8 Additionally, core-shell rubber (CSR) particles have been utilized to improve fracture toughness of epoxies.9 Both of these more established additives are investigated in this work. An emerging additive that is also evaluated here is holey graphene. This nanomaterial possesses many of the advantageous properties of graphene (excellent mechanical properties, thermal and electrical conductivity, large surface area, etc.) while also exhibiting behaviors associated with flexible, porous materials (i.e., compressibility, increased permeation, etc.). Holey graphene, HG, was synthesized by the oxidation of defect-rich sites on graphene sheets through controlled thermal expo-sure.10 It is envisioned that the porous nature of HG would allow resin penetration through the graphitic plane, resulting in better interfacial interaction and therefore better translation of the nanomaterial’s properties to the surrounding matrix.

Wohl, Christopher J↗