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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