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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 703 records · Page 39

Sodium Dodecyl Sulfate–Mediated Graphene Sensor for Electrochemical Detection of the Antibiotic Drug: Ciprofloxacin

The present study involves detecting and determining CIP by a new electrochemical sensor based on graphene (Gr) in the presence of sodium dodecyl sulfate (SDS) employing voltammetric techniques. Surface morphology studies of the sensing material were analyzed using a scanning electron microscope (SEM) and atomic force microscope (AFM). In the electroanalysis of CIP at the developed electrode, an enhanced anodic peak response was recorded, suggesting the electro-oxidation of CIP at the electrode surface. Furthermore, we evaluated the impact of the electrolytic solution, scan rate, accumulation time, and concentration variation on the electrochemical behavior of CIP. The possible electrode mechanism was proposed based on the acquired experimental information. A concentration variation study was performed using differential pulse voltammetry (DPV) in the lower concentration range, and the fabricated electrode achieved a detection limit of 2.9 × 10 -8 M. The proposed sensor detected CIP in pharmaceutical and biological samples. The findings displayed good recovery, with 93.8% for tablet analysis and 93.3% to 98.7% for urine analysis. The stability of a developed electrode was tested by inter- and intraday analysis.

36 MATERIALS SCIENCE↗

Stamping Nanoparticles onto the Electrode for Rapid Electrochemical Analysis in Microfluidics

Electrochemical analysis is an efficient way to study various materials. However, nanoparticles are challenging due to the difficulty in fabricating a uniform electrode containing nanoparticles. We developed novel approaches to incorporate nanoparticles as a working electrode (WE) in a three-electrode microfluidic electrochemical cell. Specifically, conductive epoxy was used as a medium for direct application of nanoparticles onto the electrode surface. Three approaches in this work were illustrated, including sequence stamping, mix stamping, and droplet stamping. Shadow masking was used to form the conductive structure in the WE surface on a thin silicon nitride (SiN) membrane. Two types of nanomaterials, namely cerium oxide (CeO2) and graphite, were chosen as representative nanoparticles. The as-fabricated electrodes with attached particles were characterized using atomic force microscopy (AFM) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). Electrochemical analysis was performed to verify the feasibility of these nanoparticles as electrodes. Nanomaterials can be quickly assessed for their electrochemical properties using these new electrode fabrication methods in a microfluidic cell, offering a passport for rapid nanomaterial electrochemical analysis in the future.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Studying Corrosion Using Miniaturized Particle Attached Working Electrodes and the Nafion Membrane

We developed a new approach to attach particles onto a conductive layer as a working electrode (WE) in a microfluidic electrochemical cell with three electrodes. Nafion, an efficient proton transfer molecule, is used to form a thin protection layer to secure particle electrodes. Spin coating is used to develop a thin and even layer of Nafion membrane. The effects of Nafion (5 wt% 20 wt%) and spinning rates were evaluated using multiple sets of replicates. The electrochemical performance of various devices was demonstrated. Additionally, the electrochemical performance of the devices is used to select and optimize fabrication conditions. The results show that a higher spinning rate and a lower Nafion concentration (5 wt%) induce a better performance, using cerium oxide (CeO2) particles as a testing model. The WE surfaces were characterized using atomic force microscopy (AFM), scanning electron microscopy-focused ion beam (SEM-FIB), time-of-flight secondary ion mass spectrometry (ToF-SIMS), and X-ray photoelectron spectroscopy (XPS). The comparison between the pristine and corroded WE surfaces shows that Nafion is redistributed after potential is applied. Our results verify that Nafion membrane offers a reliable means to secure particles onto electrodes. Furthermore, the electrochemical performance is reliable and reproducible. Thus, this approach provides a new way to study more complex and challenging particles, such as uranium oxide, in the future.

42 ENGINEERING↗

Microscale Electrochemical Corrosion of Uranium Oxide Particles

Understanding the corrosion of spent nuclear fuel is important for the development of long-term storage solutions. However, the risk of radiation contamination presents challenges for experimental analysis. Adapted from the system for analysis at the liquid–vacuum interface (SALVI), we developed a miniaturized uranium oxide (UO 2 )-attached working electrode (WE) to reduce contamination risk. To protect UO 2 particles in a miniatured electrochemical cell, a thin layer of Nafion was formed on the surface. Atomic force microscopy (AFM) shows a dense layer of UO 2 particles and indicates their participation in electrochemical reactions. Particles remain intact on the electrode surface with slight redistribution. X-ray photoelectron spectroscopy (XPS) reveals a difference in the distribution of U(IV), U(V), and U(VI) between pristine and corroded UO 2 electrodes. The presence of U(V)/U(VI) on the corroded electrode surface demonstrates that electrochemically driven UO 2 oxidation can be studied using these cells. Our observations of U(V) in the micro-electrode due to the selective semi-permeability of Nafion suggest that interfacial water plays a key role, potentially simulating a water-lean scenario in fuel storage conditions. This novel approach offers analytical reproducibility, design flexibility, a small footprint, and a low irradiation dose, while separating the α-effect. This approach provides a valuable microscale electrochemical platform for spent fuel corrosion studies with minimal radiological materials and the potential for diverse configurations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Towards Low-Temperature CVD Synthesis and Characterization of Mono- or Few-Layer Molybdenum Disulfide

Molybdenum disulfide (MoS 2 ) transistors are a promising alternative for the semiconductor industry due to their large on/off current ratio (>10 10 ), immunity to short-channel effects, and unique switching characteristics. MoS 2 has drawn considerable interest due to its intriguing electrical, optical, sensing, and catalytic properties. Monolayer MoS 2 is a semiconducting material with a direct band gap of ~1.9 eV, which can be tuned. Commercially, the aim of synthesizing a novel material is to grow high-quality samples over a large area and at a low cost. Although chemical vapor deposition (CVD) growth techniques are associated with a low-cost pathway and large-area material growth, a drawback concerns meeting the high crystalline quality required for nanoelectronic and optoelectronic applications. This research presents a lower-temperature CVD for the repeatable synthesis of large-size mono- or few-layer MoS 2 using the direct vapor phase sulfurization of MoO 3 . The samples grown on Si/SiO 2 substrates demonstrate a uniform single-crystalline quality in Raman spectroscopy, photoluminescence (PL), scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and scanning transmission electron microscopy. These characterization techniques were targeted to confirm the uniform thickness, stoichiometry, and lattice spacing of the MoS 2 layers. The MoS 2 crystals were deposited over the entire surface of the sample substrate. With a detailed discussion of the CVD setup and an explanation of the process parameters that influence nucleation and growth, this work opens a new platform for the repeatable synthesis of highly crystalline mono- or few-layer MoS 2 suitable for optoelectronic application.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Formation of Nano- and Micro-Scale Surface Features Induced by Long-Range Femtosecond Filament Laser Ablation

In this work, we study the characteristics of femtosecond-filament-laser–matter interactions and laser-induced periodic surface structures (LIPSS) at a beam-propagation distance up to 55 m. The quantification of the periodicity of filament-induced self-organized surface structures was accomplished by SEM and AFM measurements combined with the use of discrete two-dimensional fast Fourier transform (2D-FFT) analysis, at different filament propagation distances. The results show that the size of the nano-scale surface features increased with ongoing laser filament processing and, further, periodic ripples started to form in the ablation-spot center after irradiation with five spatially overlapping pulses. The effective number of irradiating filament pulses per spot area affected the developing surface texture, with the period of the low spatial frequency LIPSS reducing notably at a high pulse number. The high regularity of the filament-induced ripples was verified by the demonstration of the angle-of-incidence-dependent diffraction of sunlight. This work underlines the potential of long-range femtosecond filamentation for energy delivery at remote distances, with suppressed diffraction and long depth focus, which can be used in biomimetic laser surface engineering and remote-sensing applications.

36 MATERIALS SCIENCE↗

CT584 Is Not a Protective Vaccine Antigen against Respiratory Chlamydial Challenge in Mice

Background: Chlamydia trachomatis is the most prevalent bacterial sexually transmitted pathogen in humans worldwide. Since chlamydial infection is largely asymptomatic with the potential for serious complications, a preventative vaccine is likely the most viable long-term answer to this public health threat. Cell-free protein synthesis (CFPS) utilizes the cellular protein manufacturing machinery decoupled from the requirement for maintaining cellular viability, offering the potential for flexible, rapid, and decentralized production of recombinant protein vaccine antigens. Methods: Here, we use CFPS to produce the full-length putative chlamydial type three secretion system (T3SS) needle-tip protein, CT584, for evaluation as a vaccine antigen in mouse models. High-speed atomic force microscopy (HS-AFM) (RIBM, Tsukuba, Japan) imaging and computer simulations confirm that CFPS-produced CT584 retains a native-like structure prior to immunization. Female mice were primed with CT584 adjuvanted with CpG-1826 intranasally (i.n.) or CpG-1826 + Montanide ISA 720 intramuscularly (i.m.), followed four weeks later by an i.m. boost before respiratory challenge with 10 4 inclusion forming units (IFU) of Chlamydia muridarum. Results: Immunization with CT584 generated robust antibody responses but weak cell-mediated immunity and failed to protect against i.n. challenge as demonstrated by body weight loss, increased lung weights, and the presence of high numbers of IFUs in the lungs. Conclusion: While CT584 was not a protective vaccine candidate, the speed and flexibility with which CFPS can be used to produce other potential chlamydial antigens make it an attractive technique for antigen production.

60 APPLIED LIFE SCIENCES↗

Multiscale water drop contact angles at selected silica surfaces

In this paper, multiscale advancing contact angles for glycerol/water drops at silica surfaces are reported for millidrops, submicron-drops, and nanodrops. Selected silica surfaces were muscovite, silicon, and talc. The contact angles for millidrops (1–2 mm) were determined by the traditional sessile drop technique. For submicron-drops (0.1–1.0 μm), a hollow tip Atomic Force Microscope (AFM) procedure was used. The contact angles for nanodrops (~7 nm) were examined from Molecular Dynamics (MD) simulation. The results were compared to evaluate the effect of drop size on the contact angle. In the case of the hydrophobic talc surface, the 75° advancing contact angle did not vary significantly with drop size. For the hydrophilic muscovite surface, the water drop wet the surface and an advancing contact angle of about 10° was found for the millidrops and submicron-drops. However, for the MD simulated nanodrops, attachment and spreading of the ~7 nm drop created a 2D film of molecular dimensions, the contact angle of which was difficult to define and varied from 0° to 17°. Perhaps of equal interest from the MD simulation results was that the spreading of the glycerol/water nanodrop at the muscovite surface resulted in crystallographic directional transport of water molecules to the extremities of the 2D film. Such separation and segregation left the center of the film with an increased concentration of glycerol. Based on these results, the line tension, which has been found in other investigations to account for contact angle decrease with a decrease in drop size, does not seem to be a significant factor in this study.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Visualizing Solution Structure at Solid-Liquid Interfaces using Three-Dimensional Fast Force Mapping

Amongst the challenges for a variety of research fields are the visualization of solid-liquid interfaces and understanding how they are affected by the solution conditions such as ion concentrations, pH, ligands, and trace additives, as well as the underlying crystallography and chemistry. Here, in this context, three-dimensional fast force mapping (3D FFM) has emerged as a promising tool for investigating solution structure at interfaces. This capability is based on atomic force microscopy (AFM) and allows the direct visualization of interfacial regions in three spatial dimensions with sub-nanometer resolution. Here we provide a detailed description of the experimental protocol for acquiring 3D FFM data. The main considerations for optimizing the operating parameters depending on the sample and application are discussed. Moreover, the basic methods for data processing and analysis are discussed, including the transformation of the measured instrument observables into tip-sample force maps that can be linked to the local solution structure. Finally, we shed light on some of the outstanding questions related to 3D FFM data interpretation and how this technique can become a central tool in the repertoire of surface science.

Nakouzi, Elias↗

Optimizing Magnetic Force Microscopy Resolution and Sensitivity to Visualize Nanoscale Magnetic Domains

Magnetic force microscopy (MFM) enables mapping local magnetic fields across a sample surface with nanoscale resolution. To perform MFM, an atomic force microscopy (AFM) probe whose tip has been magnetized vertically (i.e., perpendicular to the probe cantilever) is oscillated at a fixed height above the sample surface. The resultant shifts in the oscillation phase or frequency, which are proportional to the magnitude and sign of the vertical magnetic force gradient at each pixel location, are then tracked and mapped. Although the spatial resolution and sensitivity of the technique increases with decreasing lift height above the surface, this seemingly straightforward path to improved MFM images is complicated by considerations such as minimizing topographical artifacts due to shorter range van der Waals forces, increasing the oscillation amplitude to further improve sensitivity, and the presence of surface contaminants (in particular water due to humidity under ambient conditions). In addition, due to the orientation of the probe's magnetic dipole moment, MFM is intrinsically more sensitive to samples with an out-of-plane magnetization vector. Here, high-resolution topographical and magnetic phase images of single and bicomponent nanomagnet artificial spin-ice (ASI) arrays obtained in an inert (argon) atmosphere glovebox with <0.1 ppm O 2 and H 2 O are reported. Further, optimization of lift height and drive amplitude for high resolution and sensitivity while simultaneously avoiding the introduction of topographical artifacts is discussed, and detection of the stray magnetic fields emanating from either end of the nanoscale bar magnets (~250 nm long and <100 nm wide) aligned in the plane of the ASI sample surface is shown. Likewise, using the example of a Ni-Mn-Ga magnetic shape memory alloy (MSMA), MFM is demonstrated in an inert atmosphere with magnetic phase sensitivity capable of resolving a series of adjacent magnetic domains each ~200 nm wide.

47 OTHER INSTRUMENTATION↗

The molecular mechanism of load adaptation by branched actin networks

Branched actin networks are self-assembling molecular motors that move biological membranes and drive many important cellular processes, including phagocytosis, endocytosis, and pseudopod protrusion. When confronted with opposing forces, the growth rate of these networks slows and their density increases, but the stoichiometry of key components does not change. The molecular mechanisms governing this force response are not well understood, so we used single-molecule imaging and AFM cantilever deflection to measure how applied forces affect each step in branched actin network assembly. Although load forces are observed to increase the density of growing filaments, we find that they actually decrease the rate of filament nucleation due to inhibitory interactions between actin filament ends and nucleation promoting factors. The force-induced increase in network density turns out to result from an exponential drop in the rate constant that governs filament capping. The force dependence of filament capping matches that of filament elongation and can be explained by expanding Brownian Ratchet theory to cover both processes. We tested a key prediction of this expanded theory by measuring the force-dependent activity of engineered capping protein variants and found that increasing the size of the capping protein increases its sensitivity to applied forces. In summary, we find that Brownian Ratchets underlie not only the ability of growing actin filaments to generate force but also the ability of branched actin networks to adapt their architecture to changing loads.

59 BASIC BIOLOGICAL SCIENCES↗

Universal aspects of brittle fracture, adhesion, and atomic force microscopy

This universal relation between binding energy and interatomic separation was originally discovered for adhesion at bimetallic interfaces involving the simple metals Al, Zn, Mg, and Na. It is shown here that the same universal relation extends to adhesion at transition-metal interfaces. Adhesive energies have been computed for the low-index interfaces of Al, Ni, Cu, Ag, Fe, and W, using the equivalent-crystal theory (ECT) and keeping the atoms in each semiinfinite slab fixed rigidly in their equilibrium positions. These adhesive energy curves can be scaled onto each other and onto the universal adhesion curve. The effect of tip shape on the adhesive forces in the atomic-force microscope (AFM) is studied by computing energies and forces using the ECT. While the details of the energy-distance and force-distance curves are sensitive to tip shape, all of these curves can be scaled onto the universal adhesion curve.

Banerjea, Amitava↗

Atomic oxygen effects on thin film space coatings studied by spectroscopic ellipsometry, atomic force microscopy, and laser light scattering

The University of Nebraska is currently evaluating Low Earth Orbit (LEO) simulation techniques as well as a variety of thin film protective coatings to withstand atomic oxygen (AO) degradation. Both oxygen plasma ashers and an electron cyclotron resonance (ECR) source are being used for LEO simulation. Thin film coatings are characterized by optical techniques including Variable Angle Spectroscopic Ellipsometry, Optical spectrophotometry, and laser light scatterometry. Atomic Force Microscopy (AFM) is also used to characterize surface morphology. Results on diamondlike carbon (DLC) films show that DLC degrades with simulated AO exposure at a rate comparable to Kapton polyimide. Since DLC is not as susceptible to environmental factors such as moisture absorption, it could potentially provide more accurate measurements of AO fluence on short space flights.

Synowicki, R. A.↗

On the typography of flight-deck documentation

Many types of paper documentation are employed on the flight-deck. They range from a simple checklist card to a bulky Aircraft Flight Manual (AFM). Some of these documentations have typographical and graphical deficiencies; yet, many cockpit tasks such as conducting checklists, way-point entry, limitations and performance calculations, and many more, require the use of these documents. Moreover, during emergency and abnormal situations, the flight crews' effectiveness in combating the situation is highly dependent on such documentation; accessing and reading procedures has a significant impact on flight safety. Although flight-deck documentation are an important (and sometimes critical) form of display in the modern cockpit, there is a dearth of information on how to effectively design these displays. The object of this report is to provide a summary of the available literature regarding the design and typographical aspects of printed matter. The report attempts 'to bridge' the gap between basic research about typography, and the kind of information needed by designers of flight-deck documentation. The report focuses on typographical factors such as type-faces, character height, use of lower- and upper-case characters, line length, and spacing. Some graphical aspects such as layout, color coding, fonts, and character contrast are also discussed. In addition, several aspects of cockpit reading conditions such as glare, angular alignment, and paper quality are addressed. Finally, a list of recommendations for the graphical design of flight-deck documentation is provided.

Degani, Asaf↗

Low earth simulation and materials characterization

Oxygen plasma ashers and an electron cyclotron resonance (ECR) sources are currently being used for low Earth orbit (LEO) simulation. The suitability of each of these simulation techniques is considered. Thin film coatings are characterized by optical techniques, including variable-angle spectroscopic ellipsometry, optical spectrophotometry, and laser light scatterometry. Atomic force microscopy (AFM) has been used to characterize the surface morphology of thin aluminum films as a function of substrate temperature during deposition. Results on diamondlike carbon (DLC) films show that DLC degrades with simulated atomic oxygen (AO) exposure at a rate comparable to Kapton polyimide. Since DLC is not as susceptible as Kapton to environmental factors such as moisture absorption, it could potentially provide more accurate measurements of AO fluence on short space flights.

Synowicki, R. A.↗

X-ray scattering measurements from thin foil X-ray mirrors

Thin foil X-ray mirrors are to be used as the reflecting elements in the telescopes of the X-ray satellites Spectrum-X-Gamma (SRG) and ASTRO-D. High resolution X-ray scattering measurements from the Au coated and dip-lacquered Al foils are presented. These were obtained from SRG mirrors positioned in a test quadrant of the telescope structure and from ASTRO-D foils held in a simple fixture. The X-ray data is compared with laser data and other surface structure data such as STM, atomic force microscopy (AFM), TEM, and electron micrography. The data obtained at Cu K-alpha(1), (8.05 keV) from all the mirrors produced on Al foils shows a scatter which limits the obtainable half-power width to above 1.5 arcmin. Mirrors based on electroformed Ni foils, however, show local regions with a factor of 4 better performance, and they are being developed for future applications.

Christensen, F. E.↗

JOVE NASA-FIT program: Microgravity and aeronomy projects

This semi-annual status report is divided into two sections: Scanning Tunneling Microscopy Lab and Aeronomy Lab. The Scanning Tunneling Microscopy (STM) research involves studying solar cell materials using the STM built at Florida Tech using a portion of our initial Jove equipment funding. One result of the participation in the FSEC project will be to design and build an STM system which is portable. This could serve as a prototype STM system which might be used on the Space Shuttle during a Spacelab mission, or onboard the proposed Space Station. The scanning tunneling microscope is only able to image the surface structure of electrically conductive crystals; by building an atomic force microscope (AFM) the surface structure of any sample, regardless of its conductivity, will be able to be imaged. With regards to the Aeronomy Lab, a total of four different mesospheric oxygen emission codes were created to calculate the intensity along the line of sight of the shuttle observations for 2972A, Herzberg I, Herzberg II, and Chamberlain bands. The thermosphere-ionosphere coupling project was completed with two major accomplishments: collection of 500 data points on modulation of neutral wind with geophysical variables, and establishment of constraints on behavior of the height of the ionosphere as a result of interaction between geophysical and geometrical factors. The magnetotail plasma project has been centered around familiarization with the subject in the form of a literature search and preprocessing of IMP-8 data.

Patterson, James D.↗

Self contamination effects in the TAUVEX UV Telescope: Ground testing and computer simulation

The contamination effects due to outgassing from construction materials of the TAUVEX (Tel Aviv University UV Telescope) were evaluated using a combination of ground testing and computer simulations. Tests were performed from the material level of the system level including: (1) High sensitivity CVCM(10(exp -3 percent) measurements of critical materials. (2) Optical degradation measurements of samples specially contaminated by outgassing products at different contamination levels. (3) FTIR studies of chemical composition of outgassed products on above samples. (4) High resolution AFM studies of surface morphology of contaminated surfaces. The expected degradation of TAUVEX performance in mission was evaluated applying a computer simulation code using input parameters determined experimentally in the above tests. The results have served as guidelines for the proper selection of materials, cleanliness requirements, determination of the thermal conditions of the system and bakeout processes.

Lifshitz, Y.↗