FY2010 - Oak Ridge National Laboratory

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Seed Money Fund— Materials Science and Technology Division Mission Relevance DOE is strongly promoting transportation electrification, which is critical for reducing the nation’s dependence on oil and reducing emissions. The future of electric vehicles largely depends upon the development of battery technologies. Lithium-ion batteries have shown the best potential, but their energy and power densities are far from adequate; therefore, technical breakthroughs are urgently needed. This project will develop novel silicon micro/nanowires-based anode materials that, if successfully developed, are expected to significantly increase the capacity and power density for lithium-ion batteries. The technology, if successful, will potentially increase the charge capacity and power density for lithiumion batteries and benefit other federal agencies such as the Department of Transportation and the Department of Defense, including Army, Navy, Air Force, Defense Advanced Research Projects Agency, and Defense Threat Reduction Agency. Results and Accomplishments In FY 2010 we successfully fabricated copper-silicon core-shell nanowire arrays. The nanowires are several micrometers long with shell diameters of 300–350 nm and core diameters of 150–200 nm. Raman spectroscopy examination indicated that the silicon shells are primarily in the amorphous phase, which is preferred for the anode application. First, a couple of two-electrode coin-type half-cells have been assembled for the copper-silicon nanowire arrays. Galvanostatic cycling was carried out in a potential range of 2.0–0.005 V using a constant current charge–discharge protocol at rates from C/30 to 10C. The initial testing results are very encouraging: (1) great potential for high capacity—the capacity for the first two cells reached ~1000 mAh/g, already 3 the theoretical capacity of a conventional graphite anode, and the capacity can be further increased by increasing the Si/Cu ratio with the potential up to 3000 mAh/g; (2) excellent capacity retention with 95% after 39 cycles at various charge–discharge rates; (3) insignificant capacity drop for a higher charge–discharge rate up to 1C due to the highly conductive copper core; and (4) near 100% coulombic efficiency after the first cycle. No silicon pulverization or core-shell delamination was detected under scanning electron microscopy after 50+ charge–discharge cycles. The planned work for FY 2011 includes (1) improvement on the nanowire distribution and morphology, (2) reduction of SiO x on the nanowire surface to decrease the irreversible capacity, (3) characterizations of the nonstructural and compositional evolutions induced by lithium-ion insertion–extraction, and (4) further electrochemical evaluation using half-cell and/or full-cell configurations. 05866 Synthesis of High-Performance Lignin-Derived Biothermoplastics Rebecca H. Brown, Tomonori Saito, Deanna L. Pickel, Joseph M. Pickel, Frederick S. Baker, and Amit K. Naskar Project Description Lignin is the second most abundant natural polymer, accounting for up to 30% by weight of wood. Lignin is a valuable by-product of the paper and pulp industry that is currently utilized in a variety of low-value applications and as fuel for the paper mills. The overarching intent of this project is to establish chemical synthetic routes for producing lignin-based thermoplastics, which will increase the value of lignin by-products. Today’s available lignin-based bioplastics are primarily thermosets, and therefore nonrecyclable. This project aims to move well beyond current state-of-the-art lignin products 222
Seed Money Fund— Materials Science and Technology Division and demonstrate the capability to synthesize inexpensive and high toughness biothermoplastics from biomass lignin feedstocks. The specific objectives are (1) characterization of lignin residues from multiple commercial biomass sources; (2) prepolymerization of lignin to produce higher molecular weight polymer precursors; (3) synthesis of thermoplastics and thermoplastic elastomers from selected lignins; and (4) determination of structure-property relationships of lignin-derived bioplastics. The development of new value-added lignin products may lead to significant enhancement to the economics of ethanol production in future biorefineries. Mission Relevance Significant potential for development of lignin biomass feedstocks as value-added products exists, and such development relies on the identification of new markets for this valuable natural biopolymer. Although research is being conducted at ORNL to produce materials from lignin, including carbon fibers and nanoporous carbons for energy storage sponsored by the DOE Office of Energy Efficiency and Renewable Energy, none is focused on the development of high performance thermoplastics from lignin. The successful development of lignin-based thermoplastics will allow for the manufacture of fully biobased composite materials to complement efforts in lignin-based carbon fibers. Additionally, the development of new value-added lignin products will impact the economics of ethanol production in biorefineries, a major focus area of the BioEnergy Science Center at ORNL. Additionally, sustainable biopolymers are an area of interest for the <strong>National</strong> Science Foundation and the Department of Agriculture. The U.S. chemical, automotive, and aircraft industries will benefit through improved competitiveness, sustainability, and energy efficiency in processes and products. Results and Accomplishments During FY 2010 chemical synthesis routes to the formation of lignin-based thermoplastics were demonstrated. Through careful tuning of reaction conditions, higher molecular weight lignin fractions were achieved through a chemical reaction while maintaining solubility in tetrahydrofuran and alkaline solution. A significant increase in glass transition temperature (T g ) from 107°C to greater than 160°C occurred due to changes in lignin structure. These fractions of higher molecular weight lignin were then used in a series of grafting reactions to form links to other pre-polymers that have soft segments. The synthesized block copolymer product is a thick, sticky brown solid, a hybrid of the dark brown powder lignin and clear viscous liquid rubber. The viscosity and shear modulus of the lignin-rubber copolymer increased by two orders of magnitude over the neat polymer soft segment or a blend of both components, proving that chemical bonding did occur. At the highest lignin content obtained, shear thinning behavior was observed in the synthesized copolymer. The invention was elected to be pursued by the ORNL Technology Transfer Group, and the patent filing process is under way. While much progress has been made, continued studies are necessary to achieve sufficient mechanical properties for use of lignin-based copolymers as industrial thermoplastics. Information Shared Mielenz, J. R., F. S. Baker, A. K. Naskar, C. C. Eberle, R. E. Norris, Jr., and J. M. Pickel. 2009. “Genetically Modified Lignin-Derived Bio-Thermoplastics for Polymer Matrix Composites.” UT-Battelle Invention Disclosure 200902293. Patent application in preparation. 223
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FY2010 - Oak Ridge National Laboratory

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