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DOE OSTI2019

Enhanced Tunability of Gold Nanoparticle Size, Spacing, and Shape for Large-Scale Plasmonic Arrays

Gold nanoparticles are important constituents in plasmonic arrays, lending themselves to electronic, optical, biomedical, sensing, and catalytic applications, among numerous others. Process variables that must be controlled when engineering plasmonic nanoparticle ensembles include nanoparticle size, shape, and spatial distribution on surfaces. The challenge in generating arrays of nanoparticles with control over these three parameters increases dramatically as spatial requirements for uniformity extend to larger processing areas. In this paper, we present a procedure that exploits thermally driven solid-state diffusional dewetting to yield considerable flexibility in generating ensembles of gold nanoparticles. Such submelting dewetting introduces fine control over particle spatial features that are currently difficult to achieve through conventional methods of generating nanoparticle arrays. Because of the simplicity of the process and its area-scalability, solid-state diffusional dewetting is shown here to be a method that could be easily scaled up to apply to large-area plasmonic fabrication processes.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Rapid sensing of hidden objects and defects using a single-pixel diffractive terahertz sensor

Abstract Terahertz waves offer advantages for nondestructive detection of hidden objects/defects in materials, as they can penetrate most optically-opaque materials. However, existing terahertz inspection systems face throughput and accuracy restrictions due to their limited imaging speed and resolution. Furthermore, machine-vision-based systems using large-pixel-count imaging encounter bottlenecks due to their data storage, transmission and processing requirements. Here, we report a diffractive sensor that rapidly detects hidden defects/objects within a 3D sample using a single-pixel terahertz detector, eliminating sample scanning or image formation/processing. Leveraging deep-learning-optimized diffractive layers, this diffractive sensor can all-optically probe the 3D structural information of samples by outputting a spectrum, directly indicating the presence/absence of hidden structures or defects. We experimentally validated this framework using a single-pixel terahertz time-domain spectroscopy set-up and 3D-printed diffractive layers, successfully detecting unknown hidden defects inside silicon samples. This technique is valuable for applications including security screening, biomedical sensing and industrial quality control.

Li, Jingxi (ORCID:0000000165958680)↗

DOE OSTI2016

Empirically testing vaterite structural models using neutron diffraction and thermal analysis

Otoliths, calcium carbonate (CaCO 3 ) ear bones, are among the most commonly used age and growth structures of fishes. Most fish otoliths are comprised of the most dense CaCO 3 polymorph, aragonite. Sturgeon otoliths, in contrast, have been characterized as the rare and structurally enigmatic polymorph, vaterite a metastable polymorph of CaCO 3 . Vaterite is an important material ranging from biomedical to personal care applications although its crystal structure is highly debated. We characterized the structure of sturgeon otoliths using thermal analysis and neutron powder diffraction, which is used non-destructively. We confirmed that while sturgeon otoliths are primarily composed of vaterite, they also contain the denser CaCO 3 polymorph, calcite. For the vaterite fraction, neutron diffraction data provide enhanced discrimination of the carbonate group compared to x-ray diffraction data, owing to the different relative neutron scattering lengths, and thus offer the opportunity to uniquely test the more than one dozen crystal structural models that have been proposed for vaterite. Of those, space group P6 5 22 model, a = 7.1443(4)Å , c = 25.350(4)Å , V = 1121.5(2)Å 3 provides the best fit to the neutron powder diffraction data, and allows for a structure refinement using rigid carbonate groups.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2014

A solvent replenishment solution for managing evaporation of biochemical reactions in air-matrix digital microfluidics devices

Digital microfluidics (DMF) is a powerful technique for sample preparation and analysis for a broad range of biological and chemical applications. In many cases, it is desirable to carry out DMF on an open surface, such that the matrix surrounding the droplets is ambient air. However, the utility of the air-matrix DMF format has been severely limited by problems with droplet evaporation, especially when the droplet-based biochemical reactions require high temperatures for long periods of time. We present a simple solution for managing evaporation in air-matrix DMF: just-in-time replenishment of the reaction volume using droplets of solvent. We demonstrate that this solution enables DMF-mediated execution of several different biochemical reactions (RNA fragmentation, first-strand cDNA synthesis, and PCR) over a range of temperatures (4–95 °C) and incubation times (up to 1 h or more) without use of oil, humidifying chambers, or off-chip heating modules. Reaction volumes and temperatures were maintained roughly constant over the course of each experiment, such that the reaction kinetics and products generated by the air-matrix DMF device were comparable to those of conventional benchscale reactions. As a result, this simple yet effective solution for evaporation management is an important advance in developing air-matrix DMF for a wide variety of new, high-impact applications, particularly in the biomedical sciences.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Trifluoromethylation of graphene

We demonstrate trifluoromethylation of graphene by copper-catalyzed free radical reaction. The covalent addition of CF{sub 3} to graphene, which changes the carbon atom hybridization from sp{sup 2} to sp{sup 3}, and modifies graphene in a homogeneous and nondestructive manner, was verified with Raman spectroscopy, atomic force microscopy, and X-ray photoelectron spectroscopy. X-ray photoelectron spectroscopy reveals that CF{sub 3} groups are grafted to the basal plane of graphene, with about 4 at. % CF{sub 3} coverage. After trifluoromethylation, the average resistance increases by nearly one order of magnitude, and an energy gap of about 98 meV appears. The noninvasive and mild reaction to synthesize trifluoromethylated graphene paves the way for graphene's applications in electronics and biomedical areas.

36 MATERIALS SCIENCE↗

DOE OSTI2014

An enzymatic biosensor based on three-dimensional ZnO nanotetrapods spatial net modified AlGaAs/GaAs high electron mobility transistors

We designed and constructed three dimensional (3D) zinc oxide Nanotetrapods (T-ZnOs) modified AlGaAs/GaAs high electron mobility transistors (HEMTs) for enzymatic uric acid (UA) detection. The chemical vapor deposition synthesized T-ZnOs was distributed on the gate areas of HEMTs in order to immobilize uricase and improve the sensitivity of the HEMTs. Combining with the high efficiency of enzyme immobilization by T-ZnOs and high sensitivity from HEMT, the as-constructed uricase/T-ZnOs/HEMTs biosensor showed fast response towards UA at ∼1 s, wide linear range from 0.2 nM to 0.2 mM and the low detect limit at 0.2 nM. The results point out an avenue to design electronic device as miniaturized lab-on-chip device for high sensitive and specific in biomedical and clinical diagnosis applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

Metallic and porous Ti nanorod arrays for visible-IR light absorption and dendrite-free stable lithium-metal batteries

It is still a challenging task to prepare highly porous nanorod arrays of metals formed on substrates for optical and energy storage applications. Herein, we demonstrate the design and synthesis of black color, metallic and highly porous Ti nanorod arrays as novel current collectors for dendrite-free and highly stable Li-metal anodes. The high porosity of metallic nanorod arrays provides numerous heterogeneous nucleation sites and huge contact area and large space for the accommodation of Li metal. The conductive metallic Ti nanorod arrays enhance electrode integration. Effectively, it eliminates formation Li dendrites and demonstrates superior cycling stability over 300 cycles. Additionally, the unique porous structures of the nanorod arrays can decrease the amplitude of forced vibration in narrow space leading to light absorption. Interestingly, the metal is black instead of metallic color. The black metallic nanorod arrays can absorb more than 96% of both visible and infra-red lights. Furthermore, this black color metallic porous nanorod arrays may find additional applications in aerospace, energy, biomedical, defence, and chemical industries.

25 ENERGY STORAGE↗

DOE OSTI2023

Ti-6Al-4V to over 1.2 TPa: Shock Hugoniot experiments, ab initio calculations, and a broad-range multiphase equation of state

Titanium alloys are used in a large array of applications. In this work we focus our attention on the most used alloy, Ti-6Al-4V (Ti64), which has excellent mechanical and biocompatibility properties with applications in aerospace, defense, biomedical, and other fields. Here we present high-fidelity experimental shock compression data measured on Sandia’s Z machine. We extend the principal shock Hugoniot for Ti64 to more than threefold compression, up to over 1.2 TPa. We use the data to validate our ab initio molecular dynamics simulations and to develop a highly reliable, multiphase equation of state (EOS) for Ti64, spanning a broad range of temperature and pressures. The first-principles simulations show very good agreement with Z data and with previous three-stage gas gun data from Sandia’s STAR facility. The resulting principal Hugoniot and the broad-range EOS and phase diagram up to 10 TPa and 10 5 K are suitable for use in shock experiments and in hydrodynamic simulations. The high-precision experimental results and high-fidelity simulations demonstrate that the Hugoniot of the Ti64 alloy is stiffer than that of pure Ti and reveal that Ti64 melts on the Hugoniot at a significantly lower pressure and temperature than previously modeled.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2015

The clinical impact of recent advances in LC-MS for cancer biomarker discovery and verification

Mass spectrometry-based proteomics has become an indispensable tool in biomedical research with broad applications ranging from fundamental biology, systems biology, and biomarker discovery. Recent advances in LC-MS have made it become a major technology in clinical applications, especially in cancer biomarker discovery and verification. To overcome the challenges associated with the analysis of clinical samples, such as extremely wide dynamic range of protein concentrations in biofluids and the need to perform high throughput and accurate quantification, significant efforts have been devoted to improve the overall performance of LC-MS bases clinical proteomics. In this review, we summarize the recent advances in LC-MS in the aspect of cancer biomarker discovery and quantification, and discuss its potentials, limitations, and future perspectives.

Environmental Molecular Sciences Laboratory↗

DOE OSTI2025

Oxidative Funneling of PVDC (CRADA Final Report)

Poly(vinylidene chloride) (PVDC) is a major polymer product from the Participant. PVDC-containing plastics are not commonly recycled. To overcome the challenges associated with recycling PVDC and multi-layer materials, we propose a tandem catalytic-biological process to convert PVDC containing waste to upcycled, tunable products such as polyhydroxyalkanoates (PHAs). PHAs are commercially relevant, biodegradable polymers that are useful in packaging, biomedical, and personal care applications. This technology, which the Contractor has named oxidative funneling (OxFun), uses a metal-promoted autoxidation step to depolymerize co-mingled polymers to a mixture of oxygenated compounds, which an engineered bacterium can funnel to a single bioproduct: here, medium chain length polyhydroxyalkanoates (mcl-PHAs). The proposed oxidation chemistry is amenable to inclusion of additional polymers, and the biocatalyst can be engineered to convert the deconstruction products to a variety of valuable chemicals, thus presenting a tunable system for both feedstock variability and target product. Pseudomonas putida KT2440 – a metabolically robust microbe that has been engineered and proven viable for upcycling deconstructed polystyrene (PS), high density polyethlene (HDPE), and polyethylene terephthalate (PET) – can be engineered with enzymes capable of de-chlorinating PVDC deconstruction products (e.g., 2,2-dichloroacetate) in addition to PE-derived substrates into mcl-PHAs.

36 MATERIALS SCIENCE↗

NASA NTRS1984

Transmitting Electromagnetic Energy into Liquids

Rough liquid surface enhances coupling. Agitating surface of liquid nitrogen bath with periodic or aperiodic excitation enhances electromagnetic coupling between microwave horn and blackbody temperature standard immersed in liquid. Useful in interfaces between electromagnetic radiation and liquids. Biomedical, radar, and meteorological applications.

Johnston, E. J.↗

NASA NTRS1991

Video Image Communication And Retrieval - Updated

Video Image Communication and Retrieval (VICAR) package of computer programs is general-purpose image-processing software system. Intended for processing data from Jet Propulsion Laboratory's unmanned planetary spacecraft, now used in variety of other applications, including processing of biomedical images, cartography, studies of Earth resources, and geological exploration. Development of newest version of VICAR emphasizes standardized, easily-understood user interface, shield between user and host operating system, and comprehensive array of image-processing capabilities.

Wall, Ray J.↗

NASA NTRS1990

The BIMDA shuttle flight mission - A low cost MPS payload

The design, operation, and experimental protocol of the Bioserve-ITA Materials Dispersion Apparatus Payload (BIMDA) to be flown on the Space Shuttle on STS-37 are described. The aim of BIMDA is to investigate the methods and commercial potential of biomedical and fluid science applications in the microgravity environment. The BIMDA payload operations are diagrammed, and the payload components and experiments are listed, including the investigators and sponsoring institutions.

Holemans, Jaak↗

NASA NTRS1994

Computer Program Helps Enhance Images

Pixel Pusher is Macintosh application program for viewing and performing minor enhancements on imagery. Works with color images digitized to 8 bits. Reads image files in JPL's two primary image formats VICAR and PDS as well as in Macintosh PICT format. VICAR (NPO-18076) handles array of image-processing capabilities used for variety of applications, including processing of biomedical images, cartography, imaging of Earth resources, and geological exploration. Pixel Pusher also imports color lookup tables in VICAR format for viewing images in pseudocolor (256 colors). Written in Symantec's Think C.

Stanfill, Daniel F., IV↗

NASA NTRS1995

Improved Solid-State Microanemometer

Improved solid-state microanemometer suitable for measuring flows in variety of biomedical, industrial, and other applications. Small size, unique design, and one-piece construction provides combination of short response time, structural rigidity, optimal dissipation of heat, and versatility in application. Device includes four integral sensing resistors exposed to flow measured and serves as hot-film anemometer subunits. Sensing resistors connected to external excitation-and-measurement circuits operating in any of standard hot-film-anemometer modes; constant input voltage, constant input current, or constant resistance with feedback.

Henderson, H. Thurman↗

NASA NTRS2009

Adaptive Morphological Feature-Based Object Classifier for a Color Imaging System

Utilizing a Compact Color Microscope Imaging System (CCMIS), a unique algorithm has been developed that combines human intelligence along with machine vision techniques to produce an autonomous microscope tool for biomedical, industrial, and space applications. This technique is based on an adaptive, morphological, feature-based mapping function comprising 24 mutually inclusive feature metrics that are used to determine the metrics for complex cell/objects derived from color image analysis. Some of the features include: Area (total numbers of non-background pixels inside and including the perimeter), Bounding Box (smallest rectangle that bounds and object), centerX (x-coordinate of intensity-weighted, center-of-mass of an entire object or multi-object blob), centerY (y-coordinate of intensity-weighted, center-of-mass, of an entire object or multi-object blob), Circumference (a measure of circumference that takes into account whether neighboring pixels are diagonal, which is a longer distance than horizontally or vertically joined pixels), . Elongation (measure of particle elongation given as a number between 0 and 1. If equal to 1, the particle bounding box is square. As the elongation decreases from 1, the particle becomes more elongated), . Ext_vector (extremal vector), . Major Axis (the length of a major axis of a smallest ellipse encompassing an object), . Minor Axis (the length of a minor axis of a smallest ellipse encompassing an object), . Partial (indicates if the particle extends beyond the field of view), . Perimeter Points (points that make up a particle perimeter), . Roundness [(4(pi) x area)/perimeter(squared)) the result is a measure of object roundness, or compactness, given as a value between 0 and 1. The greater the ratio, the rounder the object.], . Thin in center (determines if an object becomes thin in the center, (figure-eight-shaped), . Theta (orientation of the major axis), . Smoothness and color metrics for each component (red, green, blue) the minimum, maximum, average, and standard deviation within the particle are tracked. These metrics can be used for autonomous analysis of color images from a microscope, video camera, or digital, still image. It can also automatically identify tumor morphology of stained images and has been used to detect stained cell phenomena (see figure).

McDowell, Mark↗

NASA NTRS2013

Improved Cell Culture Method for Growing Contracting Skeletal Muscle Models

An improved method for culturing immature muscle cells (myoblasts) into a mature skeletal muscle overcomes some of the notable limitations of prior culture methods. The development of the method is a major advance in tissue engineering in that, for the first time, a cell-based model spontaneously fuses and differentiates into masses of highly aligned, contracting myotubes. This method enables (1) the construction of improved two-dimensional (monolayer) skeletal muscle test beds; (2) development of contracting three-dimensional tissue models; and (3) improved transplantable tissues for biomedical and regenerative medicine applications. With adaptation, this method also offers potential application for production of other tissue types (i.e., bone and cardiac) from corresponding precursor cells.

Marquette, Michele L.↗

DOE OSTI2019

Characterizing The Mechanical Properties of Polyurethane Foams

The purpose is to determine the mechanical properties of polyurethane foams with the intent of using PU foams to fill large void asymmetrical volumes like a glovebox to fixate transferable radiological material. Testing the resiliency of foam technologies when exposed to physicals stressors will be done. Six COTS PU foams considered will be fabricated and tested (iT 7, iT 8, iT 14, iT 23, 3M Fire Barrier, and Hilti) with and without additives at 12.5% wt (Bi, WO{sub 3}, and Na{sub 2}WO{sub 3}). Polyurethanes (PU) are a special class of polymeric materials that have great potential in many applications. Used in automotive, biomedical, construction, and textiles industries. Sought after due to its versatility and superior properties. PU foams have become one of the most prominent PU-based products. Bench-scale testing by SRNL and FIU-ARC confirmed PU foam technology's superior capabilities: Cured in various and desired volumes; No samples generated heat above 90 deg. C during curing reaction; Incorporation of additives (Bi, WO{sub 3}, BiO{sub 3}, Na{sub 2}WO{sub 3}) led to the following shielding: 98% of Am-241, 16% of Cs-137, 9.5% of Co-60. Proved foams' resistance to thermal stressors: Foams lasted 2 hours of direct flame; Excellent thermal insulation; Maintained structural integrity; No smoke or flame propagation. Experiment 1: A tensile tester (MTS Criterion Series 43) will be utilize to evaluate various properties of different PU rigid and flexible foams with and without additives (at 12.5% wt) under tension at 1 mm/s. Experiment 2: A thermogravimetric analysis (TGA) and Dynamic Mechanical Analyzer (DMA) will be employed to determine PU foams' breakdown of physical properties while under a constant heat rate (10 C/min) and strain rate (1%) under a period of time. Foams with additives showed an increase in stiffness and durability during tensile testing with WO{sub 3} producing the best results for Foam iT 7. All the other foam samples showed similar trends. Glass transition temperature (Tg) range for Foam iT 7 with Na{sub 2}WO{sub 3} ranged from 120-150 C while Foam iT 7 blank Tg range was from 90-110 C with a difference of about 30 C showing improvement with addition of additives.

36 MATERIALS SCIENCE↗