Publications

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As alternative energy generating devices (i.e., solar, wind, etc) are added onto the electrical energy grid (AC grid), irregularities in the available electricity due to natural occurrences (i.e., clouds reducing solar input or wind burst increasing wind powered turbines) will be dramatically increased. Due to their almost instantaneous response, modern flywheel-based energy storage devices can act a mechanical mechanism to regulate the AC grid; however, improved spin speeds will be required to meet the necessary energy levels to balance these green energy variances. Focusing on composite flywheels, we have investigated methods for improving the spin speeds based on materials needs. The so-called composite flywheels are composed of carbon fiber (C-fiber), glass fiber, and a glue (resin) to hold them together. For this effort, we have focused on the addition of fillers to the resin in order to improve its properties. Based on the high loads required for standard meso-sized fillers, this project investigated the utility of ceramic nanofillers since they can be added at very low load levels due to their high surface area. The impact that TiO2 nanowires had on the final strength of the flywheel material was determined by a three-point-bend test. The results of the introduction of nanomaterials demonstrated an increase in strength of the flywheels C-fiber-resin moiety, with an upper limit of a 30% increase being reported. An analysis of the economic impact concerning the utilization of the nanowires was undertaken and after accounting for new-technology and additional production costs, return on improved-nanocomposite investment was approximated at 4-6% per year over the 20-year expected service life. Further, it was determined based on the 30% improvement in strength, this change may enable a 20-30% reduction in flywheel energy storage cost ($/kW-h).

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This report addresses recent developments concerning the identification and handling of potential peroxide forming (PPF) and peroxide yielded derivative (PYD) chemicals. PPF chemicals are described in terms of labeling, shelf lives, and safe handling requirements as required at SNL. The general peroxide chemistry concerning formation, prevention, and identification is cursorily presented to give some perspective to the generation of peroxides. The procedure for determining peroxide concentrations and the proper disposal methods established by the Hazardous Waste Handling Facility are also provided. Techniques such as neutralization and dilution are provided for the safe handling of any PYD chemicals to allow for safe handling. The appendices are a collection of all available SNL documentation pertaining to PPF/PYD chemicals to serve as a single reference.

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The first step in an attempt to isolate Sco from a Wo crucible was explored by soaking the samples in a series of organic (HOAc) and inorganic (HCl, H2SO4, H3PO4, HNO3) acids. All samples, except the HOAc, yielded a powder. The weight loss suggests that HNO3 is the most efficient solvent; however, the powders were tentatively identified by PXRD and found to contain both W and Sc by-products. The higher weight loss may also indicate dissolution of the Wo crucible, which was further evidenced upon visual inspection of the crucible. The H3PO4 acid soak yielded the cleanest removal of Sc from the crucible. More work to understand the separation of the Sco from the Wo crucible is necessary but the acid routes appear to hold promise under not as of yet established criteria.

Lithium iron double aryloxides ([Li2Fe(OAr)4]) were synthesized, characterized, and investigated for use as precursors to LiFeO 2 nanomaterials. From the reaction of iron mesityl, two equivalents of lithium bis(trimethylsilyl) amide, and a series of monosubstituted [HOC 6H4(R)-2 where R = CH3 (oMP), CH(CH 3)2 (oPP), C(CH3)3 (oBP)] or disubstituted [HOC6H3(R)2-2,6 where R = CH 3 (DMP), CH(CH3)2 (DIP), C(CH3) 3 (DBP), C6H5 (DPhP)] aryl alcohols (H-OAr) in tetrahydrofuran (THF) or pyridine (py) were isolated. The mixed-cation Li-Fe precursors that were successfully isolated from this reaction were crystallographically identified as the double aryloxides [Fe((μ-OAr) 2Li(solv)2)2] (OAr = oPP: solv = THF (1), py (2); DMP/THF (3)) and the unusual salt [Li(THF)4][Fe(DBP) 3] (4). For the other OAr/solvent systems investigated, previously published Li or Fe alkoxide compounds or oils were isolated. Compounds 1-4 were further characterized using a variety of analytical methods but the paramagnetic nature of the Fe prevented NMR analyses. The mixed-cation precursors were used for production of nanomaterials following a solvothermal route using dioxane (in place of THF) or pyridine as the solvent. The final materials generated were characterized as the substituted lithium iron oxide structure (LiFeO 2; PDF 01-073-6306). Attempts to cycle the Li in these materials failed to demonstrate appreciable mobile capacity at reasonable potentials; however, a capacity of 87 mAh/g that quickly faded during cycling was observed at very low potentials (start: ∼0.6 V; end: 0.5 V versus Li). © 2013 Elsevier Ltd. All rights reserved.

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During this task, Silane functionalized TiO2 and HK3Ti4O4(SiO4)3 were sent to Goodyear (GY) for testing. These materials were characterized based on their interaction with the model elastomer, squalene. The Van der Waals interactions and Hamaker Constants for ZnO particles in squalene and rubber materials were characterized and it was determined that a 10-20 nm spacing was necessary between primary filler particles to maintain a stable nanocomposite. Contact angle measurements on the ZnO and ZnO-silane materials indicated that the solvent should wet the particles, and solvophobic attractions should not be present. These studies showed that the surface modification with sulfosilane coupling agents was successful, and high levels of dispersion of the particles remained possible. Further, a novel surface charging phenomenon where negative surface charging is developed in the squalene environment was observed and corroborated by measurements of particle size and of the surface modified materials in squalene. This impacts the dispersion of the particles according to the traditional colloidal interpretation of electrostatic repulsive forces between particles. Additionally, thin nanocomposite fibers were developed using electrospinning. The size and shape of the oxides did not change during the electrospinning process, although the shape of the fiber and the distribution of the particles, particularly for ZnO, was not ideal. There was an obvious increase in elastic modulus and hardness from the addition of the oxides, but differentiating the oxides, and particularly the surfactants, was difficult. The A-1289 lead to the greatest dispersion of the filler particles, while the A-1589 and the NXT produced clustered particle aggregates. This agrees with previous study of these materials in low molecular weight squalene solvent studies reported earlier. The behavior of the nanoparticle ZnO and the microparticle silica is different as well, with the ZnO being contained within the elastomer, and the SiO2 forming monolayers at the surface of the elastomer. The dynamic mechanical analysis did not show clear trends between the surface modification and the aggregate structure. In the silica particles, the NXT led to the least particle interaction, followed by the A-1289 and highest particle interaction found for the A-1589. For the nanosized ZnO, the best dispersion was found for the A-1589, with both the A-1289 and NXT exhibiting frequency dependent responses.

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