Publications

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This report summarizes accomplishments of a three-year project focused on developing technical capabilities for measuring and modeling neuronal processes at the nanoscale. It was successfully demonstrated that nanoprobes could be engineered that were biocompatible, and could be biofunctionalized, that responded within the range of voltages typically associated with a neuronal action potential. Furthermore, the Xyce parallel circuit simulator was employed and models incorporated for simulating the ion channel and cable properties of neuronal membranes. The ultimate objective of the project had been to employ nanoprobes in vivo, with the nematode C elegans, and derive a simulation based on the resulting data. Techniques were developed allowing the nanoprobes to be injected into the nematode and the neuronal response recorded. To the authors's knowledge, this is the first occasion in which nanoparticles have been successfully employed as probes for recording neuronal response in an in vivo animal experimental protocol.

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We report the initial use of lithographically defined carbon growth templates for use as an epitaxial lateral overgrowth (ELOG) mask for metalorganic chemical vapor deposition (MOCVD) heteroepitaxial GaN on sapphire. Interferometric lithography is used to define high aspect ratio structures in SU-8, which are then pyrolyzed in a reducing atmosphere up to 1200 °C. The resist structures convert to amorphous carbon, shrinking 80% in the vertical direction and 53% in the horizontal direction, but maintain their pattern geometry and adhesion to the substrate. These templates are capable of surviving GaN nucleation layer growth temperatures (∼530 °C), GaN crystal growth and high-temperature annealing up to 1050 °C. This new approach to ELOG offers several advantages, requiring fewer processing steps, and favorable selectivity tendencies as well as the capability to create growth masks which are difficult or impossible to fabricate using a top-down etching approach. © 2008 Elsevier B.V. All rights reserved.

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This senior council Tier 1 LDRD was focused on exploring the use of porous growth masks as a method for defect reduction during heteroepitaxial crystal growth. Initially our goal was to investigate porous silica as a growth mask, however, we expanded the scope of the research to include several other porous growth masks on various size scales, including mesoporous carbon, photolithographically patterned SU-8 and carbonized SU-8 structures. Use of photolithographically defined growth templates represents a new direction, unique in the extensive literature of patterned epitaxial growth, and presents the possibility of providing a single step growth mask. Additional research included investigation of pore viability via electrochemical deposition into high aspect ratio photoresist. This project was a small footprint research effort which, nonetheless, produced significant progress towards both the stated goal as well as unanticipated research directions.

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We report a synthesis of FePt nanorods by confining decomposition of Fe(CO)5 and reduction of Pt(caca)2 in surfactant reverse cylindrical micelles. The controlled nucleation and growth kinetics in confined environment allows easy control over Fe/Pt composition, nanorod uniformity, and nanorod aspect ratio. The FePt nanorods tend to self-assemble into ordered arrays along three-dimensions. Directed assembly under external magnetic field leads to two-dimensional ordered arrays, parallel to the substrate magnetic field. We expect that with optimized external magnetic fields, we should be able to assemble these nanorods into orientated one or two-dimensional arrays, providing a uniform anisotropic magnetic platform for varied applications in enhanced data storage, magneto-electron transport, etc. Copyright © 2007 American Chemical Society.

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This LDRD program was directed towards the development of a portable micro-nuclear magnetic resonance ({micro}-NMR) spectrometer for the detection of bioagents via induced amplification of solvent relaxation based on superparamagnetic nanoparticles. The first component of this research was the fabrication and testing of two different micro-coil ({micro}-coil) platforms: namely a planar spiral NMR {micro}-coil and a cylindrical solenoid NMR {micro}-coil. These fabrication techniques are described along with the testing of the NMR performance for the individual coils. The NMR relaxivity for a series of water soluble FeMn oxide nanoparticles was also determined to explore the influence of the nanoparticle size on the observed NMR relaxation properties. In addition, The use of commercially produced superparamagnetic iron oxide nanoparticles (SPIONs) for amplification via NMR based relaxation mechanisms was also demonstrated, with the lower detection limit in number of SPIONs per nanoliter (nL) being determined.

This one-year out-of-the-box LDRD was focused on exploring the use of porous growth masks as a method for defect reduction during heteroepitaxial crystal growth. Initially our goal was to investigate porous silica as a growth mask, however, we expanded the scope of the research to include several other porous growth masks on various size scales, including mesoporous carbon, and the UV curable epoxy, SU-8. Use of SU-8 as a growth mask represents a new direction, unique in the extensive literature of patterned epitaxial growth, and presents the possibility of providing a single step growth mask. Additional research included investigation of pore viability via electrochemical deposition into high aspect ratio photoresist patterns and pilot work on using SU-8 as a DUV negative resist, another significant potential result. While the late start nature of this project pushed some of the initial research goals out of the time table, significant progress was made. 3 Acknowledgements This work was performed in part at the Nanoscience @ UNM facility, a member of the National Nanotechnology Infrastructure Network, which is supported by the National Science Foundation (Grant ECS 03-35765). Sandia is multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United Stated Department of Energy's National Nuclear Security Administration under Contract DE-AC04-94AL85000. This work was supported under the Sandia LDRD program (Project 99405). 4

A gecko's extraordinary ability to suspend itself from walls and ceilings of varied surface roughness has interested humans for hundreds of years. Many theories and possible explanations describing this phenomenon have been proposed including sticky secretions, microsuckers, and electrostatic forces; however, today it is widely accepted that van der Waals forces play the most important role in this type of dry adhesion. Inarguably, the vital feature that allows a gecko's suspension is the presence of billions 3 of tiny hairs on the pad of its foot called spatula. These features are small enough to reach within van der Waals distances of any surface (spatula radius %7E100 nm); thus, the combined effect of billions of van der Waals interactions is more than sufficient to hold a gecko's weight to surfaces such as smooth ceilings or wet glass. Two lithographic approaches were used to make hierarchal structures with dimensions similar to the gecko foot dimensions noted above. One approach combined photo-lithography with soft lithography (micro-molding). In this fabrication scheme the fiber feature size, defined by the alumina micromold was 0.2 um in diameter and 60 um in height. The second approach followed more conventional photolithography-based patterning. Patterned features with dimensions %7E0.3 mm in diameter by 0.5 mm tall were produced. We used interfacial force microscopy employing a parabolic diamond tip with a diameter of 200 nm to measure the surface adhesion of these structures. The measured adhesive forces ranged from 0.3 uN - 0.6 uN, yielding an average bonding stress between 50 N/cm2 to 100 N/cm2. By comparison the reported literature value for the average stress of a Tokay gecko foot is 10 N/cm2. Acknowledgements This work was funded by Sandia National Laboratory's Laboratory Directed Research & Development program (LDRD). All coating processes were conducted in the cleanroom facility located at the University of New Mexico's Center for High Technology Materials (CHTM). SEM images were performed at UNM's Center for Micro-Engineering on equipment funded by a NSF New Mexico EPSCoR grant. 4

Our discovery that the introduction of living cells (Saccharomyces cerevisiae) alters dramatically the evaporation driven self-assembly of lipid-silica nanostructures suggested the formation of novel bio/nano interfaces useful for cellular interrogation at the nanoscale. This one year ''out of the box'' LDRD focused on the localization of metallic and semi-conducting nanocrystals at the fluid, lipid-rich interface between S. cerevisiae and the surrounding phospholipid-templated silica nanostructure with the primary goal of creating Surface Enhanced Raman Spectroscopy (SERS)-active nanostructures and platforms for cellular integration into electrode arrays. Such structures are of interest for probing cellular responses to the onset of disease, understanding of cell-cell communication, and the development of cell-based bio-sensors. As SERS is known to be sensitive to the size and shape of metallic (principally gold and silver) nanocrystals, various sizes and shapes of nanocrystals were synthesized, functionalized and localized at the cellular surface by our ''cell-directed assembly'' approach. Laser scanning confocal microscopy, SEM, and in situ grazing incidence small angle x-ray scattering (GISAXS) experiments were performed to study metallic nanocrystal localization. Preliminary Raman spectroscopy studies were conducted to test for SERS activity. Interferometric lithography was used to construct high aspect ratio cylindrical holes on patterned gold substrates and electro-deposition experiments were performed in a preliminary attempt to create electrode arrays. A new printing procedure was also developed for cellular integration into nanostructured platforms that avoids solvent exposure and may mitigate osmotic stress. Using a different approach, substrates comprised of self-assembled nanoparticles in a phospholipid templated silica film were also developed. When printed on top of these substrates, the cells integrate themselves into the mesoporous silica film and direct organization of the nanoparticles to the cell surface for integration into the cell.

The ability of semiconductor nanocrystals (NCs) to display multiple (size-specific) colors simultaneously during a single, long term excitation holds great promise for their use in fluorescent bio-imaging. The main challenges of using nanocrystals as biolabels are achieving biocompatibility, low non-specific adsorption, and no aggregation. In addition, functional groups that can be used to further couple and conjugate with biospecies (proteins, DNAs, antibodies, etc.) are required. In this project, we invented a new route to the synthesis of water-soluble and biocompatible NCs. Our approach is to encapsulate as-synthesized, monosized, hydrophobic NCs within the hydrophobic cores of micelles composed of a mixture of surfactants and phospholipids containing head groups functionalized with polyethylene glycol (-PEG), -COOH, and NH{sub 2} groups. PEG provided biocompatibility and the other groups were used for further biofunctionalization. The resulting water-soluble metal and semiconductor NC-micelles preserve the optical properties of the original hydrophobic NCs. Semiconductor NCs emit the same color; they exhibit equal photoluminescence (PL) intensity under long-time laser irradiation (one week) ; and they exhibit the same PL lifetime (30-ns). The results from transmission electron microscopy and confocal fluorescent imaging indicate that water-soluble semiconductor NC-micelles are biocompatible and exhibit no aggregation in cells. We have extended the surfactant/lipid encapsulation techniques to synthesize water-soluble magnetic NC-micelles. Transmission electron microscopy results suggest that water-soluble magnetic NC-micelles exhibit no aggregation. The resulting NC-micelles preserve the magnetic properties of the original hydrophobic magnetic NCs. Viability studies conducted using yeast cells suggest that the magnetic nanocrystal-micelles are biocompatible. We have demonstrated, for the first time, that using external oscillating magnetic fields to manipulate the magnetic micelles, we can kill live cells, presenting a new magnetodynamic therapy without side effects.

Highly ordered gold nanocrystal (NC)/silica films are synthesized by self-assembly of water-soluble gold NC micelles and silica using a sol-gel spin coating technique. The optical properties are analyzed using ellipsometry and ultraviolet-visible spectroscopy. Transmission and absorption spectra were measured for wavelengths ranging from 200 to 2000 nm. The absorption spectra show a strong surface plasmon absorption band at {approx}520 nm for all samples. Charge transport behavior of the films was examined using metal-oxide-semiconductor (MOS) and metal-insulator-metal (MIM) structures. MOS capacitor samples exhibit charge storage with discharge behavior dominated by electron transport within the gold NC arrays. Low temperature current-voltage measurements on MIM devices reveal electrical conduction with a thermal activation energy of {approx}90 meV. For temperatures less than 100 K, the I-V characteristics of the NC film exhibits a strong coulomb blockade effect, with a threshold voltage of {approx}0.5 V measured at 78 K.

We report a simple, rapid approach to synthesize water-soluble and biocompatible fluorescent quantum dot (QD) micelles by encapsulation of monodisperse, hydrophobic QDs within surfactant/lipid micelles. Analyses of UV-vis and photo luminescence spectra, along with transmission electron microscopy, indicate that the water-soluble semiconductor QD micelles are monodisperse and retain the optical properties of the original hydrophobic QDs. The QD micelles were shown to be biocompatible and exhibited little or no aggregation when taken up by cultured rat hippocampal neurons.