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DOE OSTI2025

Evaluating the Origins of Aerobic Oxidation Catalysis with TAM-3, a MOF with Accessible Co(II) Sites and Large Pores

Metal-organic frameworks (MOFs) are attractive platforms that merge concepts of homogeneous and heterogeneous catalysis. Catalyst design and optimization are enabled by an array of synthetic methods that offer independent control over the local chemical structure of lattice-embedded metal ions (i.e., ligand identity and geometry) and the long-range materials properties (i.e., porosity). Establishing the origin of catalytic activity in MOF-promoted reactions remains a significant challenge: The relative rates of catalyst turnover and substrate diffusion dictate the extent to which interstitial sites are accessible and operational in catalysis. To minimize the contributions of surface sites in catalysis, materials with large pore dimensions are often sought, however, the impact of pore expansion on the origins of catalytic activity is similarly challenging to establish. Here, we describe TAM-3, a Co(II) based MOF with accessible metal sites supported by a facially coordinating tris-tetrazole ligand set. TAM-3 features large channel-like pores (17 × 23 Å) and promotes aerobic C−H oxidation and olefin epoxidation. Using a set of simple kinetics experiments, based on the analysis of kinetic isotope effects and olefin oxidation diastereoselectivities, we demonstrate that despite the large pores, interstitial metal ions do not significantly contribute to the observed substrate oxidation. This study highlights the importance of conducting kinetic experiments to assess the origin of apparent catalytic activity with MOFs and the challenge of harnessing reactive oxidants with microporous catalyst materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Coaxial color channel focus evaluation to estimate standoff height in directed energy deposition additive manufacturing

Directed energy deposition (DED) is an additive manufacturing process that is being rapidly adopted by industry and is well suited for the fabrication of complex components in a variety of metal alloys. In laser cladding systems such as DED, powder is blown in a stream to a metal substrate coincident with a laser necessary to deposit molten metal with 3D spatial control. The focus of both the laser and the powder stream are crucial, and best deposition occurs at a predetermined standoff height between the build surface and the print head. Generally, no monitoring of this distance is implemented in commercial DED systems. Due to potential over or under building, the standoff height often changes over time but tends to self-correct. However, inexpensive and minimally intrusive methods to identify optimal standoff are required to provide real-time control to maintain the optimal distance. The present work explores the quantification of the focus of the three-color channels of a coaxial camera to determine the standoff height. An experiment was performed in which a 254 mm wall is built and the standoff height, initially 5.0 mm below the optimal position, was then intentionally increased every 25.4 mm of wall length by an amount of 1.0 mm to a final position 7.0 mm above optimal. Computer vision is demonstrated to monitor the amount of focus in each color band and estimate standoff distance. Finally, a response can be calculated in under 40 ms using simple hardware and can work in most laser-based DED systems.

36 MATERIALS SCIENCE↗

NASA NTRS2013

Mathematical Models of the Common-Source and Common-Gate Amplifiers using a Metal-Ferroelectric-Semiconductor Field effect Transistor

Mathematical models of the common-source and common-gate amplifiers using metal-ferroelectric- semiconductor field effect transistors (MOSFETs) are developed in this paper. The models are compared against data collected with MOSFETs of varying channel lengths and widths, and circuit parameters such as biasing conditions are varied as well. Considerations are made for the capacitance formed by the ferroelectric layer present between the gate and substrate of the transistors. Comparisons between the modeled and measured data are presented in depth as well as differences and advantages as compared to the performance of each circuit using a MOSFET.

Hunt, Mitchell↗

NASA NTRS2006

Multichannel X-Band Dielectric-Resonator Oscillator

A multichannel dielectric-resonator oscillator (DRO), built as a prototype of a local oscillator for an X-band transmitter or receiver, is capable of being electrically tuned among and within 26 adjacent frequency channels, each 1.16 MHz wide, in a band ranging from 7,040 to 7,070 GHz. The tunability of this oscillator is what sets it apart from other DROs, making it possible to use mass-produced oscillator units of identical design in diverse X-band applications in which there are requirements to use different fixed frequencies or to switch among frequency channels. The oscillator (see figure) includes a custom-designed voltage-controlled-oscillator (VCO) monolithic microwave integrated circuit (MMIC), a dielectric resonator disk (puck), and two varactor-coupling circuits, all laid out on a 25-mil (0.635-mm)-thick alumina substrate having a length and width of 17.8 mm. The resonator disk has a diameter of 8.89 mm and a thickness of 4.01 mm. The oscillator is mounted in an 8.9-mm-deep cavity in a metal housing. The VCO MMIC incorporates a negative- resistance oscillator amplifier along with a buffer amplifier. The resonator disk is coupled to a microstrip transmission line connected to the negative-resistance port of the VCO MMIC. The two varactor-coupling circuits include microstrip lines, laid out orthogonally to each other, for coupling with the resonator disk. Each varactor microstrip line is DC-coupled to an external port via a microwave choke. One varactor is used for coarse tuning to select a channel; the other varactor is used (1) for fine tuning across the 1.16-MHz width of each channel and (2) as a feedback port for a phase-lock loop. The resonator disk is positioned to obtain (1) the most desirable bandwidth, (2) relatively tight coupling with the microstrip connected to the coarse-tuning varactor, and (3) relatively loose coupling with the microstrip connected to the fine-tuning varactor. Measurements of performance showed that the oscillator can be switched among any of the 26 channels and can be phase-locked to a nominal frequency in any channel. The degree of nonlinearity of tuning was found not to exceed 2.5 percent. The tuning sensitivity was found to be 6.15 MHz/V at a bias offset of -2 V on the phase-lock-loop varactor. The phase noise of the oscillator in free-running operation was found to be -107 dBc/Hz (where dBc signifies decibels relative to the carrier signal) at 100 kHz away from the carrier frequency.

Mysoor, Narayan↗

DOE OSTI2021

The fluoride permeation pathway and anion recognition in Fluc family fluoride channels

Fluc family fluoride channels protect microbes against ambient environmental fluoride by undermining the cytoplasmic accumulation of this toxic halide. These proteins are structurally idiosyncratic, and thus the permeation pathway and mechanism have no analogy in other known ion channels. Although fluoride-binding sites were identified in previous structural studies, it was not evident how these ions access aqueous solution, and the molecular determinants of anion recognition and selectivity have not been elucidated. Using x-ray crystallography, planar bilayer electrophysiology, and liposome-based assays, we identified additional binding sites along the permeation pathway. We used this information to develop an oriented system for planar lipid bilayer electrophysiology and observed anion block at one of these sites, revealing insights into the mechanism of anion recognition. We propose a permeation mechanism involving alternating occupancy of anion-binding sites that are fully assembled only as the substrate approaches.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2025

Diode effect for skyrmions interacting with linear protrusion defects

We simulate collectively interacting skyrmions in a channel with periodic asymmetry, and find a strong diode effect for the skyrmion flow. There is also an asymmetry in the skyrmion annihilation rate for currents applied along the hard or easy substrate asymmetry direction, with a higher annihilation rate for hard direction currents. We map out the diode efficiency as a function of magnetic field and substrate asymmetry angle. We also show that the Magnus force impacts the diode motion and annihilation rate asymmetry by forcing skyrmions into corners of the protrusion geometry.

36 MATERIALS SCIENCE↗

NASA NTRS1998

Alignment and Polarization Sensitivity Study for the Cassini-Composite InfraRed Spectrometer (CIRS) Far InfraRed (FIR) Interferometer

The Composite InfraRed Spectrometer (CIRS) instrument flying on the Cassini spacecraft to Saturn is a cryogenic spectrometer with far-infrared (FIR) and mid-infrared (MIR) channels. The CIRS FIR channel is a polarizing interferometer that contains three polarizing grid components. These components are an input polarizer, a polarizing beamsplitter, and an output polarizer/analyzer. They consist of a 1.5 micron thick mylar substrate with 2 gm wide copper wires, with 2 gm spacing (4 micron pitch) photolithographically deposited on the substrate. This paper details the polarization sensitivity studies performed on the output polarizer/analyzer, and the alignment sensitivity studies performed on the input polarizer and beamsplitter components in the FIR interferometer.

Crooke, Julie A.↗

NASA NTRS1998

Alignment and Polarization Sensitivity Study on the Cassini: CIRS FIR Interferometer

The Composite InfraRed Spectrometer (CIRS) instrument flying on the Cassini spacecraft to Saturn is a cryogenic spectrometer with far-infrared (FIR) and mid-infrared (MIR) channels. The CIRS FIR channel is a polarizing interferometer that contains three polarizing grid components. These components are an input polarizer, a polarizing beamsplitter, and an output polarizer/analyzer. They consist of a 1.5 micron thick mylar substrate with 2 microns wide copper wires, with 2 microns spacing (4 microns pitch) photolithographically deposited on the substrate. This paper details the alignment sensitivity studies performed on the polarizing beamsplitter, and the polarization sensitivity studies performed on all three polarizing components in the FIR interferometer.

Crooke, Julie↗

NASA NTRS2006

FETs Based on Doped Polyaniline/Polyethylene Oxide Fibers

A family of experimental highly miniaturized field-effect transistors (FETs) is based on exploitation of the electrical properties of nanofibers of polyaniline/ polyethylene oxide (PANi/PEO) doped with camphorsulfonic acid. These polymer-based FETs have the potential for becoming building blocks of relatively inexpensive, low-voltage, highspeed logic circuits that could supplant complementary metal oxide/semiconductor (CMOS) logic circuits. The development of these polymerbased FETs offers advantages over the competing development of FETs based on carbon nanotubes. Whereas it is difficult to control the molecular structures and, hence, the electrical properties of carbon nanotubes, it is easy to tailor the electrical properties of these polymerbased FETs, throughout the range from insulating through semiconducting to metallic, through choices of doping levels and chemical manipulation of polymer side chains. A further advantage of doped PANi/PEO nanofibers is that they can be made to draw very small currents and operate at low voltage levels, and thus are promising for applications in which there are requirements to use many FETs to obtain large computational capabilities while minimizing power demands. Fabrication of an experimental FET in this family begins with the preparation of a substrate as follows: A layer of silicon dioxide between 50 and 200 nm thick is deposited on a highly doped (resistivity 0.01 W.cm) silicon substrate, then gold electrodes/contact stripes are deposited on the oxide. Next, one or more fibers of camphorsulphonic acid-doped PANi/PEO having diameters of the order of 100 nm are electrospun onto the substrate so as to span the gap between the gold electrodes (see Figure 1). Figure 2 depicts measured current-versus-voltage characteristics of the device of Figure 1, showing that saturation channel currents occur at source-todrain potentials that are surprisingly low, relative to those of CMOS FETs. The hole mobility in the depletion regime in this transistor was found to be 1.4 10(exp -4) sq cm/(V.s), while the one-dimensional charge density at zero gate bias was estimated to be approximately one hole per 50 two-ring repeat units of polyaniline, consistent with the rather high channel conductivity (approx. 10(exp -3) S/cm). Reducing or eliminating the PEO content of the fibers is expected to enhance the properties of future versions of this transistor.

Theofylaktos, Noulie↗

NASA NTRS2006

Nano Sensors for Gas Detection in Space and Ground Support Applications

Personnel living in a space environment as well as technicians and engineers preparing spacecraft for launch can potentially be exposed to small amounts of hazardous gases. It is therefore important to be able to detect, identify and quantify the presence of a gas especially when its presence could lead to a fatal situation. The use of small and sensitive sensors can allow for the placement of these devices over a large area, thus allowing for a more precise and timely determination of a gas leak. ASRC Aerospace and its research partners are developing nano sensors for detection of various gases, including but not limited to: H2, NH3, N2O4, hydrazine and others. Initial laboratory testing has demonstrated the capability to detect the gases in concentrations lower than parts per million. Testing and development is continuing to improve the response and recovery times, to increase the sensitivity of the devices. Different coatings and electrodes are currently being evaluated to determine the optimum configuration of a variety of gases. The small footprint of the Nano sensors allows for several devices, each responsive in a different way to different gases, to be placed into a single substrate. Multiple devices embedded into a single substrate results in increased reliability and in a decrease for periodic calibrations. The use of different coatings will result in a small electronic nose capable of distinguishing between different gases. A multi-channel signal conditioner amplifier built on a small multi chip module is used to process the output of the sensors and to deliver a signal that can be remotely monitored. All the data is digitized and transmitted over the same cable pair used to power the amplifier. Multiple outputs can be connected to a single cable pair in order to minimize the added weight and expense associated with cabling in a spacecraft. The sensors will be run through a qualification process to evaluate their suitability for space applications we are expecting to have fully functional sensors available for initial field deployment and testing by the end of the year 2006.

Medelius, Pedro J.↗

NASA NTRS2019

Applications of Atomic Layer Deposition in the Modification of Carbon Nanotubes

Atomic Layer Deposition (ALD) is a cost-effective nanoadditive-manufacturing technique that allows for conformal coating of substrates with atomic control in a benign temperature and pressure environment. Using paired precursor gases, thin films can be deposited on flat or textured surfaces ranging from glass, polymers, aerogels, and metals. Through atomic layer control, where single layers of atoms are deposited, fabrication of metal transparent films, nano-laminates, and coatings of nano-channels and pores is achievable. Reaction mechanisms in ALD are normally self-limiting, allowing for atomically accurate control of nanometer (nm) thicknesses. Therefore, high uniformity and precise thickness control make ALD an attractive process for the creation of novel nano-scale devices. Decreases in resistivity and density of electrical wire are needed to improve the function of electronics, electric motors and cables. Such improvements may be accomplished by adding ballistically conducting, metallic carbon nanotubes (CNT) to Cu. ALD was used to coat multiple substrates including CNT with Cu in an effort to make CNT-Cu composites which is more conductive and less dense than Cu. In addition, ALD can be used to as a method to deposit the catalyst layer seed layer for CNT growth using Ni. The ALD of copper metallic films can follow multiple reaction pathways depending on the ALD precursors used. For this work the reaction pathway was deposition of copper oxide and then post process annealing in a hydrogen environment. Copper(II) diacetylacetonate (Cu(acac)2) and ozone are used as precursors for copper oxide. As-deposited copper oxide films prepared at 180°C resulted in a growth per cycle of 1.0 A/cycle with low film resistivity.

Dwivedi, Vivek H.↗

DOE OSTI2022

Bilayer hybrid graphite anodes via freeze tape casting for extreme fast charging applications

Extreme fast charging (XFC) of lithium-ion batteries is critical for continuous market adoption of electric vehicles. However, mass transport limitations and sluggish kinetics lead to lithium plating in graphite anodes under fast charging conditions. One approach to address the mass transport limitation in graphite is to design low-tortuosity electrodes to enhance ionic transport. In this study, a bilayer hybrid structured electrode with directionally aligned channels was developed via freeze tape casting, which enables faster lithium ion diffusion through the graphite electrode. A scalable roll-to-roll process was designed in which slurry can be cast on any substrates for simple processing. Additionally, electrochemical impedance spectroscopy measurements indicated that the bilayer hybrid coating had both low tortuosity and short diffusion pathways, enabling XFC charging. Rate testing for the bilayer hybrid electrode indicated superior performance over the other coatings, exhibiting a ~20% improvement in the charge capacity compared with the conventional coating at 5C and 10 min total charging time. The bilayer hybrid electrode also demonstrated a 10% improvement in capacity retention compared with the conventional electrode after 1000 cycles at XFC conditions. This study demonstrates freeze tape casting as a scalable way to fabricate low-tortuosity electrodes for XFC applications.

25 ENERGY STORAGE↗

DOE OSTI2021

High performance ionic-liquid-gated air doped diamond field-effect transistors

Here we report successful fabrication of high performance ion-gated field-effect transistors (FETs) on hydrogenated diamond surface. Investigations on the hydrogen (H)-terminated diamond by Hall effect measurements shows Hall mobility as high as ~200 cm 2 V –1 s –1 . In addition we demonstrate a rapid fabrication scheme for achieving stable high performance devices useful for determining optimal growth and fabrication conditions. We achieved H-termination using hydrogen plasma treatment with a sheet resistivity as low as ~1.3 kΩ/sq. Conductivity through the FET channel is studied as a function of bias voltage on the liquid ion-gated electrode from –3.0 to 1.5 V. Stability of the H-terminated diamond surface was studied by varying the substrate temperature up to 350 °C. It was demonstrated that the sheet resistance and carrier densities remain stable over 3 weeks in ambient air atmosphere even at substrate temperatures up to 350 °C, whereas increasing temperature beyond this limit has effected hydrogenation. This study opens new avenues for carrying out fundamental research on diamond FET devices with ease of fabrication and high throughput.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2020

Enabling Highly Stable Li–O 2 Batteries with Full Discharge–Charge Capability: The Porous Binder- and Carbon-Free IrNi Nanosheet Cathode

Rechargeable aprotic Li-O 2 batteries have drawn much attention in light of their ultrahigh theoretical energy density. However, the sluggish kinetics of oxygen cathode reactions lead to huge energy loss, while the unfavorable side reactions associated with the widely used carbon and binder account for fast battery decay during cycles. In this work, hierarchically holey IrNi alloy nanosheets are facilely designed on Ni foam substrate as a freestanding, binder- and carbon-free cathode to address these challenges. The IrNi nanosheets consist of numerous interconnected nanoparticles, forming abundant nanoholes, benefiting active-site exposure. Moreover, the meso-/macropores pave channels for the transfer of oxygen and lithium ions and provide enough accommodation for the insoluble Li 2 O 2 product. The corresponding Li-O 2 batteries demonstrate low polarization and excellent cycle stability with full discharge/charge capability (up to 292 cycles at a current density of 0.2 mA cm -2 within a voltage range from 2.3 to 4.3 V). The long-term cycling performance is principally attributed to the exclusive catalytic stability of the holey IrNi nanosheets and its good compatibility with dimethyl sulfoxide-based electrolyte. Our research provides novel insights into the design of robust and freestanding porous cathodes for high energy density Li-O 2 batteries.

25 ENERGY STORAGE↗

DOE OSTI2021

Formation of Vertically Oriented Channels during Calcination of Surfactant-Templated Titania-Doped Mesoporous Silica Thin Films

Here, the mesoporous structure development during calcination of titania-doped mesoporous silica thin films is characterized by in situ grazing-incidence small angle x-ray scattering (GISAXS). Varying amounts of titania (≤ 6 mol%) are incorporated in cetyltrimethylammonium bromide (CTAB) templated film by two methods in this study: dispersion of titania in the silica matrix, and fixing titania at the pore surface by complexation of the titania precursor with a sugar-based co-surfactant, dodecyl maltoside (C 12 G 2 ). Before calcination, films templated with only CTAB display a mesoporous structure with a mixture of in-plane 2D hexagonal and randomly oriented porous structure, while C 12 G 2 -complexed film possessed randomly oriented mesostructure only. Both methods yield a final structure of hexagonal close-packed pores orthogonally oriented to the substrate after calcination at 500 °C. This is attributed to weak Si-O-Ti bonds which allow sintering to occur at 500 °C, combined with unidirectional thermal contraction of the film in the vertical direction. Anisotropic stress and annealing of the films allows the randomly oriented pores to merge vertically and form channels with pore diameter of 2.3 ± 0.3 nm. Titania doping greater than 1% is required for this transformation in films with no C 12 G 2 surfactant used while the transformation was observed for films with C 12 G 2 complexation even at low (0.005%) titania doping, perhaps accentuated by orientational disorder introduced by the sugar surfactant.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRSDate not supplied

Development of Multilayered Coatings for Nerva-Type Graphite Fuel Elements- An Overview

“Mid-passage corrosion” (MPC) was observed in NbC and ZrC-coated graphite (Gr)-based nuclear fuels during the NERVA/Rover programs. A new multilayered coating concept was proposed to solve this problem. The concept envisions designing a compliant multilayered coatings architecture to accommodate the thermal expansion mismatch strains between the ZrC outer coating and the Gr/(U,Zr)C fuel matrix. Additionally, the coating architecture uses diffusion barriers to minimize carbon diffusion from the substrate, and hydrogen diffusion from the flowing gas stream, into the multilayer coating. The present paper provides a brief overview of the development of multilayered coatings deposited on Gr disks, as well as within the inner channels of a19-hole hexagonal rod 152.4 mm long, by chemical vapor deposition (CVD) in proof-of concept studies. The cross-sectional microstructural observations are discussed. These trials have established that it is possible to deposit multilayered coatings by CVD in 19-hole hexagonal rods similar to the NERVA fuel rod design although the quality of the coatings and the uniformity of their thicknesses require further improvement.

Multilayer coatings, graphite, nuclear thermal pro↗

NASA NTRS2006

Four-Quadrant Analog Multipliers Using G4-FETs

Theoretical analysis and some experiments have shown that the silicon-on-insulator (SOI) 4-gate transistors known as G4-FETs can be used as building blocks of four-quadrant analog voltage multiplier circuits. Whereas a typical prior analog voltage multiplier contains between six and 10 transistors, it is possible to construct a superior voltage multiplier using only four G4-FETs. A G4-FET is a combination of a junction field-effect transistor (JFET) and a metal oxide/semiconductor field-effect transistor (MOSFET). It can be regarded as a single transistor having four gates, which are parts of a structure that affords high functionality by enabling the utilization of independently biased multiple inputs. The structure of a G4-FET of the type of interest here (see Figure 1) is that of a partially-depleted SOI MOSFET with two independent body contacts, one on each side of the channel. The drain current comprises of majority charge carriers flowing from one body contact to the other that is, what would otherwise be the side body contacts of the SOI MOSFET are used here as the end contacts [the drain (D) and the source (S)] of the G4-FET. What would otherwise be the source and drain of the SOI MOSFET serve, in the G4-FET, as two junction-based extra gates (JG1 and JG2), which are used to squeeze the channel via reverse-biased junctions as in a JFET. The G4-FET also includes a polysilicon top gate (G1), which plays the same role as does the gate in an accumulation-mode MOSFET. The substrate emulates a fourth MOS gate (G2). By making proper choices of G4-FET device parameters in conjunction with bias voltages and currents, one can design a circuit in which two input gate voltages (Vin1,Vin2) control the conduction characteristics of G4-FETs such that the output voltage (Vout) closely approximates a value proportional to the product of the input voltages. Figure 2 depicts two such analog multiplier circuits. In each circuit, there is the following: The input and output voltages are differential, The multiplier core consists of four G4- FETs (M1 through M4) biased by a constant current sink (Ibias), and The G4-FETs in two pairs are loaded by two identical resistors (RL), which convert a differential output current to a differential output voltage. The difference between the two circuits stems from their input and bias configurations. In each case, provided that the input voltages remain within their design ranges as determined by considerations of bias, saturation, and cutoff, then the output voltage is nominally given by Vout = kVin1Vin2, where k is a constant gain factor that depends on the design parameters and is different for the two circuits. In experimental versions of these circuits constructed using discrete G4- FETs and resistors, multiplication of voltages in all four quadrants (that is, in all four combinations of input polarities) was demonstrated, and deviations of the output voltages from linear dependence on the input voltages were found to amount to no more than a few percent. It is anticipated that in fully integrated versions of these circuits, the deviations from linearity will be made considerably smaller through better matching of devices.

Mojarradi, Mohammad↗

NASA NTRS2011

The QWIP Focal Plane Assembly for NASA's Landsat Data Continuity Mission

The Thermal Infrared Sensor (TIRS) is a QWIP based instrument intended to supplement the Operational Land Imager (OLI) for the Landsat Data Continuity Mission (LDCM). The TIRS instrument is a dual channel far infrared imager with the two bands centered at 10.8 m and 12.0 m. The focal plane assembly (FPA) consists of three 640x512 GaAs Quantum Well Infrared Photodetector (QWIP) arrays precisely mounted to a silicon carrier substrate that is mounted on an invar baseplate. The two spectral bands are defined by bandpass filters mounted in close proximity to the detector surfaces. The focal plane operating temperature is 43K. The QWIP arrays are hybridized to Indigo ISC9803 readout integrated circuits (ROICs). Two varieties of QWIP detector arrays are being developed for this project, a corrugated surface structure QWIP and a grating surface structure QWIP. This paper will describe the TIRS system noise equivalent temperature difference sensitivity as it affects the QWIP focal plane performance requirements: spectral response, dark current, conversion efficiency, read noise, temperature stability, pixel uniformity, optical crosstalk and pixel yield. Additional mechanical constraints as well as qualification through Technology Readiness Level 6 (TRL 6) will also be discussed.

Jhabvala, M.↗