Publications

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Sandia National Laboratories sponsored a three-year internally funded Laboratory Directed Research and Development (LDRD) effort to investigate the vulnerabilities and mitigations of a high-altitude electromagnetic pulse (HEMP) on the electric power grid. The research was focused on understanding the vulnerabilities and potential mitigations for components and systems at the high voltage transmission level. Results from the research included a broad array of subtopics, covered in twenty-three reports and papers, and which are highlighted in this executive summary report. These subtopics include high altitude electromagnetic pulse (HEMP) characterization, HEMP coupling analysis, system-wide effects, and mitigating technologies.

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The magnetic susceptibility of NO_x-loaded RE-DOBDC (rare earth (RE): Y, Eu, Tb, Yb; DOBDC: 2,5-dihydroxyterephthalic acid) metal–organic frameworks (MOFs) is unique to the MOF metal center. RE-DOBDC samples were synthesized, activated, and subsequently exposed to humid NO_x. Each NO_x-loaded MOF was characterized by powder X-ray diffraction, and the magnetic characteristics were probed by using a VersaLab vibrating sample magnetometer (VSM). Lanthanide-containing RE-DOBDC (Eu, Tb, Yb) are paramagnetic with a reduction in paramagnetism upon adsorption of NO_x. Y-DOBDC has a diamagnetic moment with a slight reduction upon adsorption of NO_x. The magnetic susceptibility of the MOF is determined by the magnetism imparted by the framework metal center. The electronic population of orbitals contributes to determining the extent of magnetism and change with NO_x (electron acceptor) adsorption. Eu-DOBDC results in the largest mass magnetization change upon adsorption of NO_x due to more available unpaired f electrons. Experimental changes in magnetic moment were supported by density functional theory (DFT) simulations of NO_x adsorbed in lanthanide Eu-DOBDC and transition metal Y-DOBDC MOFs.

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This paper evaluates the performance of a novel nano-composite core inductor. In this digest, a brief explanation of the superparamagnetic magnetite nanoparticle core is given along with magnetic characterization results and simulated design parameters and dimensions. A nearly flat relative permeability (μr) of around 5 is measured for the magnetic material to 1 MHz. A synchronous buck converter with nano-composite inductor was constructed and evaluated; the converter demonstrates a 1% improvement in conversion efficiency at higher currents (4% reduction in electrical losses), compared to an identical circuit with a benchmark commercial ferrite inductor.

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Soft matter has historically been an unlikely candidate for investigation by electron microscopy techniques due to damage by the electron beam as well as inherent instability under a high vacuum environment. Characterization of soft matter has often relied on ensemble-scattering techniques. The recent development of cryogenic transmission electron microscopy (cryo-TEM) provides the soft matter community with an exciting opportunity to probe the structure of soft materials in real space. Cryo-TEM reduces beam damage and allows for characterization in a native, frozen-hydrated state, providing direct visual representation of soft structure. This article reviews cryo-TEM in soft materials characterization and illustrates how it has provided unique insights not possible by traditional ensemble techniques. Soft matter systems that have benefited from the use of cryo-TEM include biological-based “soft” nanoparticles (e.g., viruses and conjugates), synthetic polymers, supramolecular materials as well as the organic–inorganic interface of colloidal nanoparticles. We conclude that while many challenges remain, such as combining structural and chemical analyses; the opportunity for soft matter research to leverage newly developed cryo-TEM techniques continues to excite.

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Soft magnetic materials are key to the efficient operation of the next generation of power electronics and electrical machines (motors and generators). Many new materials have been introduced since Michael Faraday's discovery of magnetic induction, when iron was the only option. However, as wide bandgap semiconductor devices become more common in both power electronics and motor controllers, there is an urgent need to further improve soft magnetic materials.These improvements will be necessary to realize the full potential in efficiency, size, weight, and power of high-frequency power electronics and high-rotational speed electrical machines. Here we provide an introduction to the field of soft magnetic materials and their implementation in power electronics and electrical machines. Additionally, we review the most promising choices available today and describe emerging approaches to create even better soft magnetic materials.

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Significant reductions recently seen in the size of wide-bandgap power electronics have not been accompanied by a relative decrease in the size of the corresponding magnetic components. To achieve this, a new generation of materials with high magnetic saturation and permeability are needed. Here, we develop gram-scale syntheses of superparamagnetic Fe/FexOy core-shell nanoparticles and incorporate them as the magnetic component in a strongly magnetic nanocomposite. Nanocomposites are typically formed by the organization of nanoparticles within a polymeric matrix. However, this approach can lead to high organic fractions and phase separation; reducing the performance of the resulting material. Here, we form aminated nanoparticles that are then cross-linked using epoxy chemistry. The result is a magnetic nanoparticle component that is covalently linked and well separated. By using this 'matrix-free' approach, we can substantially increase the magnetic nanoparticle fraction, while still maintaining good separation, leading to a superparamagnetic nanocomposite with strong magnetic properties.

This article focuses on the finite element modeling of toroidal microinductors, employing first-of-its-kind nanocomposite magnetic core material and superparamagnetic iron nanoparticles covalently cross-linked in an epoxy network. Energy loss mechanisms in existing inductor core materials are covered as well as discussions on how this novel core material eliminates them providing a path toward realizing these low form factor devices. Designs for both a 2 μH output and a 500 nH input microinductor are created via the model for a high-performance buck converter. Both modeled inductors have 50 wire turns, less than 1 cm3 form factors, less than 1 Ω AC resistance, and quality factors, Q's, of 27 at 1 MHz. In addition, the output microinductor is calculated to have an average output power of 7 W and a power density of 3.9 kW/in3 by modeling with the 1st generation iron nanocomposite core material.

A method for creating nanoparticles directly from bulk metal by applying ultrasound to the surface in the presence of a two-part surfactant system is presented. Implosive collapse of cavitation bubbles near the bulk metal surface generates powerful microjets, leading to material ejection. This liberated material is captured and stabilized by a surfactant bilayer in the form of nanoparticles. The method is characterized in detail using gold, but is also demonstrated on other metals and alloys, and is generally applicable. It is shown that nanoparticles can be produced regardless of the bulk metal form factor, and the method is extended to an environmentally important problem, the reclamation of gold from an electronic waste stream.

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A magnetically active Fe3O4/poly(ethylene oxide)-block-poly(butadiene) (PEO-b-PBD) nanocomposite is formed by the encapsulation of magnetite nanoparticles with a short-chain amphiphilic block copolymer. This material is then incorporated into the self-assembly of higher order polymer architectures, along with an organic pigment, to yield biosynthetic, bifunctional optical and magnetically active Fe3O4/bacteriochlorophyll c/PEO-b-PBD polymeric chlorosomes.

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Core–shell nanostructures are promising candidates for the next generation of catalysts due to synergistic effects which can arise from having two active species in close contact, leading to increased activity. Likewise, catalysts displaying added functionality, such as a magnetic response, can have increased scientific and industrial potential. Here, Pd/Fe3O4 core–shell nanowire clusters are synthesized and applied as hydrogenation catalysts for an industrially important hydrogenation reaction: the conversion of acetophenone to 1-phenylethanol. During synthesis, the palladium nanowires self-assemble into clusters which act as a high-surface-area framework for the growth of a magnetic iron oxide shell. This material demonstrates excellent catalytic activity due to the presence of palladium while the strong magnetic properties provided by the iron oxide shell enable facile catalyst recovery.

Extensive study of photorefractive polymeric composites photosensitized with semiconductor nanocrystals has yielded data indicating that the inclusion of such nanocrystals enhances the charge-carrier mobility, and subsequently leads to a reduction in the photorefractive response time. Unfortunately, the included nanocrystals may also act as a source of deep traps, resulting in diminished diffraction efficiencies as well as reduced two beam coupling gain coefficients. Nonetheless, previous studies indicate that this problem is mitigated through the inclusion of semiconductor nanocrystals possessing a relatively narrow band-gap. Here, we fully exploit this property by doping PbS nanocrystals into a newly formulated photorefractive composite based on molecular triphenyldiamine photosensitized with C60. Through this approach, response times of 399 μs are observed, opening the door for video and other high-speed applications. It is further demonstrated that this improvement in response time occurs with little sacrifice in photorefractive efficiency, with internal diffraction efficiencies of 72% and two-beam-coupling gain coefficients of 500 cm-1 being measured. A thorough analysis of the experimental data is presented, supporting the hypothesized mechanism of enhanced charge mobility without the accompaniment of superfluous traps. It is anticipated that this approach can play a significant role in the eventual commercialization of this class of materials.

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Ternary polymer brushes consisting of polystyrene, poly(methyl methacrylate), and poly(4-vinylpyridine) have been synthesized. These brushes laterally phase separate into several distinct phases and can be tailored by altering the relative polymer composition. Self-consistent field theory has been used to predict the phase diagram and model both the horizontal and vertical phase behavior of the polymer brushes. All phase behaviors observed experimentally correlate well with the theoretical model.

Magnetic nanoparticles are the next tool in medical diagnoses and treatment in many different biomedical applications, including magnetic hyperthermia as alternative treatment for cancer and bacterial infections, as well as the disruption of biofilms. The colloidal stability of the magnetic nanoparticles in a biological environment is crucial for efficient delivery. A surface that can be easily modifiable can also improve the delivery and imaging properties of the magnetic nanoparticle by adding targeting and imaging moieties, providing a platform for additional modification. The strategy presented in this work includes multiple nitroDOPA anchors for robust binding to the surface tied to the same polymer backbone as multiple poly(ethylene oxide) chains for steric stability. This approach provides biocompatibility and enhanced stability in fetal bovine serum (FBS) and phosphate buffer saline (PBS). As a proof of concept, these polymer-particles complexes were then modified with a near infrared dye and utilized in characterizing the integration of magnetic nanoparticles in biofilms. The work presented in this manuscript describes the synthesis and characterization of a nontoxic platform for the labeling of near IR-dyes for bioimaging.

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The synthesis of well-defined nanoparticle materials has been an area of intense investigation, but size control in nanoparticle syntheses is largely empirical. Here, we introduce a general method for fine size control in the synthesis of nanoparticles by establishing steady state growth conditions through the continuous, controlled addition of precursor, leading to a uniform rate of particle growth. This approach, which we term the "xtended LaMer mechanism" allows for reproducibility in particle size from batch to batch as well as the ability to predict nanoparticle size by monitoring the early stages of growth. We have demonstrated this method by applying it to a challenging synthetic system: magnetite nanoparticles. To facilitate this reaction, we have developed a reproducible method for synthesizing an iron oleate precursor that can be used without purification. We then show how such fine size control affects the performance of magnetite nanoparticles in magnetic hyperthermia.

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The photosensitization of photorefractive polymeric composites for operation at 633 nm is accomplished through the inclusion of narrow band gap semiconductor nanocrystals composed of PbS. Unlike previous studies involving photosensitization of photorefractive polymer composites with inorganic nanocrystals, we employ an off-resonance approach where the first excitonic transition associated with the PbS nanocrystals lies at ∼1220 nm and not the wavelength of operation. Using this methodology, internal diffraction efficiencies exceeding 82%, two-beam-coupling gain coefficients of 211 cm^-1, and response times of 34 ms have been observed, representing some of the best figures of merit reported for this class of materials. These data demonstrate the ability of semiconductor nanocrystals to compete effectively with traditional organic photosensitizers. In addition to superior performance, this approach also offers an inexpensive and easy means by which to photosensitize composite materials. The photoconductive characteristics of the composites used for this study will also be considered.

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The cycling of high-capacity electrode materials for lithium-ion batteries results in significant volumetric expansion and contraction, and this leads to mechanical failure of the electrodes. To increase battery performance and reliability, there is a drive towards the use of nanostructured electrode materials and nanoscale surface coatings. As a part of the Visiting Faculty Program (VFP) last summer, we examined the ability of aluminum oxide and gold film surface coatings to improve the mechanical and cycling properties of vapor-deposited aluminum films in lithium-ion batteries. Nanoscale gold coatings resulted in significantly improved cycling behavior for the thinnest aluminum films whereas aluminum oxide coatings did not improve the cycling behavior of the aluminum films. This summer we performed a similar investigation on vapor-deposited germanium, which has an even higher theoretical capacity per unit mass than aluminum. Because the mechanism of lithium-alloying is different for each electrode material, we expected the effects of coating the germanium surface with aluminum oxide or gold to differ significantly from previous observations. Indeed, we found that gold coatings gave only small or negligible improvements in cycling behavior of germanium films, but aluminum oxide (Al₂O₃) coatings gave significant improvements in cycling over the range of film thicknesses tested.

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A wide spectrum of photonics activities Sandia is engaged in such as solid state lighting, photovoltaics, infrared imaging and sensing, quantum sources, rely on nanoscale or ultrasubwavelength light-matter interactions (LMI). The fundamental understanding in confining electromagnetic power and enhancing electric fields into ever smaller volumes is key to creating next generation devices for these programs. The prevailing view is that a resonant interaction (e.g. in microcavities or surface-plasmon polaritions) is necessary to achieve the necessary light confinement for absorption or emission enhancement. Here we propose new paradigm that is non-resonant and therefore broadband and can achieve light confinement and field enhancement in extremely small areas [~(λ/500)^2 ]. The proposal is based on a theoretical work[1] performed at Sandia. The paradigm structure consists of a periodic arrangement of connected small and large rectangular slits etched into a metal film named double-groove (DG) structure. The degree of electric field enhancement and power confinement can be controlled by the geometry of the structure. The key operational principle is attributed to quasistatic response of the metal electrons to the incoming electromagnetic field that enables non-resonant broadband behavior. For this exploratory LDRD we have fabricated some test double groove structures to enable verification of quasistatic electronic response in the mid IR through IR optical spectroscopy. We have addressed some processing challenges in DG structure fabrication to enable future design of complex sensor and detector geometries that can utilize its non-resonant field enhancement capabilities.].

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Many reactions in both chemistry and biology rely on the ability to precisely control and fix the solution concentrations of either protons or hydroxide ions. In this report, we describe the behavior of thermally programmable pH buffer systems based on the copolymerization of varying amounts of acrylic acid (AA) groups into N-isopropylacrylamide polymers. Because the copolymers undergo phase transitions upon heating and cooling, the local environment around the AA groups can be reversibly switched between hydrophobic and hydrophilic states affecting the ionization behavior of the acids. Results show that moderate temperature variations can be used to change the solution pH by two units. However, results also indicate that the nature of the transition and its impact on the pH values are highly dependent on the AA content and the degree of neutralization. © 2012 American Chemical Society.

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Devices with nano-crystalline microstructures have been shown to possess improved electrical properties. Further advantages include lower processing temperatures; however, device fabrication from nano-particles poses several challenges. This presentation describes a novel aqueous synthesis technique to produce large batch sizes with minimal waste. The precipitate is readily converted at less than 550 C to a phase pure, nano-crystalline Pb{sub 0.88} La{sub 0.12}(Zr{sub 0.70} Ti{sub 0.30}){sub 0.97} O{sub 3} powder. Complications and solutions to sample fabrication from nano-powders are discussed, including the use of glass sintering aids to improve density and further lower sintering temperatures. Finally, electrical properties are presented to demonstrate the potential benefits of nano-crystalline capacitors.

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Nano-materials have shown unique crystallite-dependent properties that present distinct advantages for dielectric applications. PLZT is an excellent dielectric material used in several applications and may benefit crystallite engineering; however complex systems such as PLZT require well-controlled synthesis techniques. An aqueous based synthesis route has been developed, using standard precursor chemicals and scalable techniques to produce large batch sizes. The synthesis will be briefly covered, followed by a more in-depth discussion of incorporating nanocrystalline PLZT into a working device. Initial electrical properties will be presented illustrating the potential benefits and associated difficulties of working with PLZT nano-materials.

The ceramic nanocomposite capacitor goals are: (1) more than double energy density of ceramic capacitors (cutting size and weight by more than half); (2) potential cost reductino (factor of >4) due to decreased sintering temperature (allowing the use of lower cost electrode materials such as 70/30 Ag/Pd); and (3) lower sintering temperature will allow co-firing with other electrical components.

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Electrodeposited aluminum films and template-synthesized aluminum nanorods are examined as negative electrodes for lithium-ion batteries. The lithium-aluminum alloying reaction is observed electrochemically with cyclic voltammetry and galvanostatic cycling in lithium half-cells. The electrodeposition reaction is shown to have high faradaic efficiency, and electrodeposited aluminum films reach theoretical capacity for the formation of LiAl (1 Ah/g). The performance of electrodeposited aluminum films is dependent on film thickness, with thicker films exhibiting better cycling behavior. The same trend is shown for electron-beam deposited aluminum films, suggesting that aluminum film thickness is the major determinant in electrochemical performance regardless of deposition technique. Synthesis of aluminum nanorod arrays on stainless steel substrates is demonstrated using electrodeposition into anodic aluminum oxide templates followed by template dissolution. Unlike nanostructures of other lithium-alloying materials, the electrochemical performance of these aluminum nanorod arrays is worse than that of bulk aluminum. ©The Electrochemical Society.

Microencapsulation is the process of placing a shell composed of a synthetic or biological polymer completely around another chemical for the purpose of delaying or slowing its release. We report that Sandia National Laboratories was interested in microencapsulating concentrated sulfuric for a specific application. Historically, acids have been encapsulated many times using various techniques. However, the encapsulation of mineral acids has proven difficult due to the lack of a shell material robust enough to prevent premature leakage of the capsule. Using the Polymer-Polymer Incompatibility (PPI) technique, we screened a variety of shell materials and found our best results were with Derakane® 411-350, an epoxy vinyl ester resin (EVER) polymer.

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The rapid autonomous detection of pathogenic microorganisms and bioagents by field deployable platforms is critical to human health and safety. To achieve a high level of sensitivity for fluidic detection applications, we have developed a 330 MHz Love wave acoustic biosensor on 36{sup o} YX Lithium Tantalate (LTO). Each die has four delay-line detection channels, permitting simultaneous measurement of multiple analytes or for parallel detection of single analyte containing samples. Crucial to our biosensor was the development of a transducer that excites the shear horizontal (SH) mode, through optimization of the transducer, minimizing propagation losses and reducing undesirable modes. Detection was achieved by comparing the reference phase of an input signal to the phase shift from the biosensor using an integrated electronic multi-readout system connected to a laptop computer or PDA. The Love wave acoustic arrays were centered at 330 MHz, shifting to 325-328 MHz after application of the silicon dioxide waveguides. The insertion loss was -6 dB with an out-of-band rejection of 35 dB. The amplitude and phase ripple were 2.5 dB p-p and 2-3{sup o} p-p, respectively. Time-domain gating confirmed propagation of the SH mode while showing suppression of the triple transit. Antigen capture and mass detection experiments demonstrate a sensitivity of 7.19 {+-} 0.74{sup o} mm{sup 2}/ng with a detection limit of 6.7 {+-} 0.40 pg/mm{sup 2} for each channel.

A molecular-scale interpretation of interfacial processes is often downplayed in the analysis of traditional water treatment methods. However, such an approach is critical for the development of enhanced performance in traditional desalination and water treatments. Water confined between surfaces, within channels, or in pores is ubiquitous in technology and nature. Its physical and chemical properties in such environments are unpredictably different from bulk water. As a result, advances in water desalination and purification methods may be accomplished through an improved analysis of water behavior in these challenging environments using state-of-the-art microscopy, spectroscopy, experimental, and computational methods.

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As electronic assemblies become more compact and increase in processing bandwidth, escalating thermal energy has become more difficult to manage. The major limitation has been nonmetallic joining using poor thermal interface materials (TIM). The interfacial, versus bulk, thermal conductivity of an adhesive is the major loss mechanism and normally accounts for an order magnitude loss in conductivity per equivalent thickness. The next generation TIM requires a sophisticated understanding of material and surface sciences, heat transport at submicron scales, and the manufacturing processes used in packaging of microelectronics and other target applications. Only when this relationship between bond line manufacturing processes, structure, and contact resistance is well-understood on a fundamental level will it be possible to advance the development of miniaturized microsystems. This report examines using thermal and squeeze-flow modeling as approaches to formulate TIMs incorporating nanoscience concepts. Understanding the thermal behavior of bond lines allows focus on the interfacial contact region. In addition, careful study of the thermal transport across these interfaces provides greatly augmented heat transfer paths and allows the formulation of very high resistance interfaces for total thermal isolation of circuits. For example, this will allow the integration of systems that exhibit multiple operational temperatures, such as cryogenically cooled detectors.

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Field-structured magnetic particle composites are an important new class of materials that have great potential as both sensors and actuators. These materials are synthesized by suspending magnetic particles in a polymeric resin and subjecting these to magnetic fields while the resin polymerizes. If a simple uniaxial magnetic field is used, the particles will form chains, yielding composites whose magnetic susceptibility is enhanced along a single direction. A biaxial magnetic field, comprised of two orthogonal ac fields, forms particle sheets, yielding composites whose magnetic susceptibility is enhanced along two principal directions. A balanced triaxial magnetic field can be used to enhance the susceptibility in all directions, and biased heterodyned triaxial magnetic fields are especially effective for producing composites with a greatly enhanced susceptibility along a single axis. Magnetostriction is quadratic in the susceptibility, so increasing the composite susceptibility is important to developing actuators that function well at modest fields. To investigate magnetostriction in these field-structured composites we have constructed a sensitive, constant-stress apparatus capable of 1 ppm strain resolution. The sample geometry is designed to minimize demagnetizing field effects. With this apparatus we have demonstrated field-structured composites with nearly 10,000 ppm strain.

Tethered supramolecular machines represent a new class of active self-assembled monolayers in which molecular configurations can be reversibly programmed using electrochemical stimuli. We are using these machines to address the chemistry of substrate surfaces for integrated microfluidic systems. Interactions between the tethered tetracationic cyclophane host cyclobis(paraquat-p-phenylene) and dissolved {pi}-electron-rich guest molecules, such as tetrathiafulvalene, have been reversibly switched by oxidative electrochemistry. The results demonstrate that surface-bound supramolecular machines can be programmed to adsorb or release appropriately designed solution species for manipulating surface chemistry.

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Iron, the most ubiquitous of the transition metals and the fourth most plentiful element in the Earths crust, is the structural backbone of our modern infrastructure. It is therefore ironic that as a nanoparticle, iron has been somewhat neglected in favor of its own oxides, as well as other metals such as cobalt, nickel, gold, and platinum. This is unfortunate, but understandable. Irons reactivity is important in macroscopic applications (particularly rusting), but is a dominant concern at the nanoscale. Finely divided iron has long been known to be pyrophoric, which is a major reason that iron nanoparticles have not been more fully studied to date. This extreme reactivity has traditionally made iron nanoparticles difficult to study and inconvenient for practical applications. Iron however has a great deal to offer at the nanoscale, including very potent magnetic and catalytic properties. Recent work has begun to take advantage of irons potential, and work in this field appears to be blossoming.

We describe the synthesis of highly magnetic iron nanoparticles using a novel surfactant, a {beta}-diketone. We have produced 6 nm iron nanoparticles with an unusually high saturation magnetization of more than 80% the value of bulk iron. Additionally, we measured a particle susceptibility of 14 (MKS units), which is far above the value possible for micron-scale spherical particles. These properties will allow for formation of composites that can be highly structured by magnetic fields.

We demonstrate through experiment and simulation that when mono-domain Fe nanoparticles are formed into chains by the application of a magnetic field, the susceptibility of the resulting structure is greatly enhanced (11.4-fold) parallel to the particle chains and is much larger than transverse to the chains. Simulations show that this significant enhancement is expected when the susceptibility of the individual particles approaches 5 in MKS units, and is due to the spontaneous magnetization of individual particle chains, which occurs because of the strong dipolar interactions. This large enhancement is only possible with nanoparticles, because demagnetization fields limit the susceptibility of a spherical multi-domain particle to 3 (MKS). Experimental confirmation of the large susceptibility enhancement is presented, and both the enhancement and the susceptibility anisotropy are found to agree with simulation. The specific susceptibility of the nanocomposite is 54 (MKS), which exceeds the highest value we have obtained for field-structured composites of multi-domain particles by a factor of four.

Tethered films of poly n-isopropylacrylamide (PNIPAM) films have been developed as materials that can be used to switch the chemistry of a surface in response to thermal activation. In water, PNIPAM exhibits a thermally-activated phase transition that is accompanied by significant changes in polymer volume, water contact angle, and protein adsorption characteristics. New synthesis routes have been developed to prepare PNIPAM films via in-situ polymerization on self-assembled monolayers. Swelling transitions in tethered films have been characterized using a wide range of techniques including surface plasmon resonance, attenuated total reflectance infrared spectroscopy, interfacial force microscopy, neutron reflectivity, and theoretical modeling. PNIPAM films have been deployed in integrated microfluidic systems. Switchable PNIPAM films have been investigated for a range of fluidic applications including fluid pumping via surface energy switching and switchable protein traps for pre-concentrating and separating proteins on microfluidic chips.