Publications

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The Proliferation Assessment (program area - Things Thin) within the Defense Systems and Assessment Investment Area desires high energy density and long-lived power sources with moderate currents (mA) that can be used as building blocks in platforms for the continuous monitoring of chemical, biological, and radiological agents. Fuel cells can be an optimum choice for a power source because of the high energy densities that are possible with liquid fuels. Additionally, power generation and fuel storage can be decoupled in a fuel cell for independent control of energy and power density for customized, application-driven power solutions. Direct methanol fuel cells (DMFC) are explored as a possible concept to develop into ultrathin or two-dimensional power sources. New developments in nanotechnology, advanced fabrication techniques, and materials science are exploited to create a planar DMFC that could be co-located with electronics in a chip format. Carbon nanotubes and pyrolyzed polymers are used as building block electrodes - porous, mechanically compliant current collectors. Directed assembly methods including surface functionalization and layer-by-layer deposition with polyelectrolytes are used to pattern, build, and add functionality to these electrodes. These same techniques are used to incorporate nanoscale selective electrocatalyst into the carbon electrodes to provide a high density of active electron transfer sites for the methanol oxidation and oxygen reduction reactions. The resulting electrodes are characterized in terms of their physical properties, electrocatalytic function, and selectivity to better understand how processing impacts their performance attributes. The basic function of a membrane electrode assembly is demonstrated for several prototype devices.

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Advances in electrochemical energy storage science require the development of new or the refinement of existing in situ probes that can be used to establish structure - activity relationships for technologically relevant materials. The drive to develop reversible, high capacity electrodes from nanoscale building blocks creates an additional requirement for high spatial resolution probes to yield information of local structural, compositional, and electronic property changes as a function of the storage state of a material. In this paper, we describe a method for deconstructing a lithium ion battery positive electrode into its basic constituents of ion insertion host particles and a carbon current collector. This model system is then probed in an electrochemical environment using a combination of atomic force microscopy and tunneling spectroscopy to correlate local activity with morphological and electronic configurational changes. Cubic spinel Li{sub 1+x}Mn{sub 2-x}O{sub 4} nanoparticles are grown on graphite surfaces using vacuum deposition methods. The structure and composition of these particles are determined using transmission electron microscopy and Auger microprobe analysis. The response of these particles to initial de-lithiation, along with subsequent electrochemical cycling, is tracked using scanning probe microscopy techniques in polar aprotic electrolytes (lithium hexafluorophosphate in ethylene carbonate:diethylcarbonate). The relationship between nanoparticle size and reversible ion insertion activity will be a specific focus of this paper.

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Erbium is known to effectively load with hydrogen when held at high temperature in a hydrogen atmosphere. To make the storage of hydrogen kinetically feasible, a thermal activation step is required. Activation is a routine practice, but very little is known about the physical, chemical, and/or electronic processes that occur during Activation. This work presents in situ characterization of erbium Activation using variable energy photoelectron spectroscopy at various stages of the Activation process. Modification of the passive surface oxide plays a significant role in Activation. The chemical and electronic changes observed from core-level and valence band spectra will be discussed along with corroborating ion scattering spectroscopy measurements.

Erbium is known to effectively load with hydrogen when held at high temperature in a hydrogen atmosphere. To make the storage of hydrogen kinetically feasible, a thermal activation step is required. Activation is a routine practice, but very little is known about the physical, chemical, and/or electronic processes that occur during Activation. This work presents in situ characterization of erbium Activation using variable energy photoelectron spectroscopy at various stages of the Activation process. Modification of the passive surface oxide plays a significant role in Activation. The chemical and electronic changes observed from core-level and valence band spectra will be discussed along with corroborating ion scattering spectroscopy measurements.

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